# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 1579185'
_audit_update_record             
;
2017-11-11 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
# start Validation Reply Form

_vrf_PLAT780_complex1            
;
PROBLEM: Coordinates do not Form a Properly Connected Set     Please Do !
RESPONSE: They do! If you extract the embedded ins file from the cif file
using shredcif, then it is evident that the three O atoms are part of a 
disordered ClO4- anion.
;
_vrf_PLAT220_complex1            
;
PROBLEM: Non-Solvent Resd 1 O Ueq(max)/Ueq(min) Range 3.1 Ratio
RESPONSE: Part of a coordinated disordered ClO4- anion 
;
_vrf_PLAT241_complex1            
;
PROBLEM: High ?MainMol? Ueq as Compared to Neighbors of O8S Check
RESPONSE: Uij for this atom is not unreasonable; its neighbours happen
to both be heavier atoms - Cl and Cu with correspondingly small Uij.
;
_vrf_PLAT242_complex1            
;
PROBLEM: Low ?MainMol? Ueq as Compared to Neighbors of Cl1S Check
RESPONSE: CL1S and O1S are well located but the three remaining O 
atoms of this ClO4- anion are disordered through rotation about the
O-Cl axis. 
;
_vrf_PLAT354_complex1            
;
PROBLEM: Short O-H (X0.82,N0.98A) O2 - H3S .. 0.71 Ang.
RESPONSE: ...
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H30 Cl4 Cu3 N10 O20'
_chemical_formula_sum            'C30 H30 Cl4 Cu3 N10 O20'
_chemical_formula_weight         1183.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   14.859(3)
_cell_length_b                   18.703(4)
_cell_length_c                   15.719(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.99(3)
_cell_angle_gamma                90
_cell_volume                     4256.6(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9553
_cell_measurement_theta_min      3.44
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_F_000             2380
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.829
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6967
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55814
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.814
_diffrn_reflns_theta_max         26.400
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4356
_reflns_number_gt                3650
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0322P)²+11.1894P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4356
_refine_ls_number_parameters     340
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0293
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.38729(2) 0.2500 0.01899(10) Uani 1 2 d S T P . .
Cu2 Cu -0.25138(2) 0.53424(2) 0.10784(2) 0.02315(9) Uani 1 1 d . . . . .
O4 O -0.25499(11) 0.42566(10) 0.10247(11) 0.0247(4) Uani 1 1 d . . . . .
N1 N -0.08136(14) 0.30772(10) 0.20805(13) 0.0204(4) Uani 1 1 d . . . . .
N3 N -0.14461(13) 0.51089(10) 0.19998(13) 0.0193(4) Uani 1 1 d . . . . .
N2 N -0.11907(13) 0.43983(10) 0.20739(13) 0.0197(4) Uani 1 1 d . . . . .
C1 C -0.16452(16) 0.32238(13) 0.15812(15) 0.0217(5) Uani 1 1 d . . . . .
O2 O -0.17199(15) 0.54055(14) 0.00448(14) 0.0386(5) Uani 1 1 d . . . . .
H2 H -0.2045 0.5250 -0.0427 0.058 Uiso 1 1 calc R U . . .
N1T N -0.37109(15) 0.55939(13) 0.03225(15) 0.0307(5) Uani 1 1 d . . . . .
C6 C -0.18380(15) 0.40078(13) 0.15291(15) 0.0201(5) Uani 1 1 d . . . . .
C8 C -0.14963(16) 0.63093(13) 0.23080(15) 0.0213(5) Uani 1 1 d . . . . .
N4 N -0.21840(14) 0.63270(11) 0.15739(14) 0.0242(4) Uani 1 1 d . . . . .
C12 C -0.25075(19) 0.69568(15) 0.12454(18) 0.0313(6) Uani 1 1 d . . . . .
H12 H -0.2996 0.6966 0.0738 0.038 Uiso 1 1 calc R U . . .
C5 C -0.04799(18) 0.24142(13) 0.22304(17) 0.0257(5) Uani 1 1 d . . . . .
C10 C -0.1455(2) 0.75846(14) 0.23568(19) 0.0337(6) Uani 1 1 d . . . . .
H10 H -0.1200 0.8018 0.2621 0.040 Uiso 1 1 calc R U . . .
C7 C -0.11536(15) 0.55811(13) 0.25921(15) 0.0197(5) Uani 1 1 d . . . . .
C4 C -0.1027(2) 0.18377(14) 0.1866(2) 0.0361(7) Uani 1 1 d . . . . .
H4 H -0.0813 0.1360 0.1975 0.043 Uiso 1 1 calc R U . . .
C9 C -0.11209(19) 0.69283(14) 0.27147(17) 0.0275(5) Uani 1 1 d . . . . .
H9 H -0.0643 0.6908 0.3230 0.033 Uiso 1 1 calc R U . . .
C2 C -0.22175(18) 0.26747(15) 0.11851(18) 0.0293(6) Uani 1 1 d . . . . .
H2A H -0.2809 0.2770 0.0823 0.035 Uiso 1 1 calc R U . . .
C11 C -0.2157(2) 0.75979(15) 0.1618(2) 0.0367(7) Uani 1 1 d . . . . .
H11 H -0.2396 0.8040 0.1367 0.044 Uiso 1 1 calc R U . . .
C3 C -0.1889(2) 0.19778(15) 0.1341(2) 0.0382(7) Uani 1 1 d . . . . .
H3 H -0.2266 0.1590 0.1081 0.046 Uiso 1 1 calc R U . . .
Cl2 Cl 0.01882(4) 0.30970(3) 0.02804(4) 0.02568(14) Uani 1 1 d . . . . .
O5S O 0.07136(15) 0.31888(13) -0.03795(14) 0.0442(5) Uani 1 1 d . . . . .
O6S O -0.07696(14) 0.30996(16) -0.01148(15) 0.0568(7) Uani 1 1 d . . . . .
O7S O 0.04290(18) 0.24353(12) 0.07265(16) 0.0521(6) Uani 1 1 d . . . . .
O8S O 0.04064(19) 0.36717(13) 0.08953(16) 0.0555(7) Uani 1 1 d . . . . .
C13 C -0.05632(17) 0.54527(14) 0.34812(16) 0.0253(5) Uani 1 1 d . . . . .
H13A H -0.0411 0.4943 0.3551 0.038 Uiso 1 1 calc R U . . .
H13B H -0.0898 0.5599 0.3923 0.038 Uiso 1 1 calc R U . . .
H13C H 0.0007 0.5732 0.3553 0.038 Uiso 1 1 calc R U . . .
C14 C -0.43818(19) 0.58014(15) -0.00899(18) 0.0324(6) Uani 1 1 d . . . . .
C15 C -0.5240(2) 0.60656(19) -0.0627(3) 0.0594(11) Uani 1 1 d . . . . .
H15A H -0.5405 0.5782 -0.1163 0.089 Uiso 1 1 calc R U . . .
H15B H -0.5165 0.6568 -0.0775 0.089 Uiso 1 1 calc R U . . .
H15C H -0.5731 0.6026 -0.0304 0.089 Uiso 1 1 calc R U . . .
H3S H -0.148(3) 0.572(2) -0.003(3) 0.069(15) Uiso 1 1 d . . . . .
Cl1S Cl -0.15395(5) -0.01274(4) 0.19929(5) 0.03958(18) Uani 1 1 d D U . . .
O1S O -0.14014(15) 0.02099(12) 0.28296(14) 0.0435(5) Uani 1 1 d D . . . .
O2SA O -0.0790(3) 0.0145(2) 0.1605(3) 0.0472(10) Uani 0.57 1 d D U P A 1
O3SA O -0.1622(4) -0.0808(2) 0.2010(4) 0.0756(16) Uani 0.57 1 d D U P A 1
O4SA O -0.2369(3) 0.0269(2) 0.1500(2) 0.0423(9) Uani 0.57 1 d D U P A 1
O2SB O -0.1512(7) 0.0240(3) 0.1269(4) 0.070(2) Uani 0.43 1 d D U P A 2
O3SB O -0.0839(4) -0.0745(3) 0.2061(4) 0.0528(14) Uani 0.43 1 d D U P A 2
O4SB O -0.2418(3) -0.0593(3) 0.1804(4) 0.0550(16) Uani 0.43 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.937(2) 2 ?
Cu1 N1 1.937(2) . ?
Cu1 N2 2.003(2) 2 ?
Cu1 N2 2.003(2) . ?
Cu2 N3 1.942(2) . ?
Cu2 N1T 1.961(2) . ?
Cu2 N4 2.017(2) . ?
Cu2 O4 2.0329(19) . ?
Cu2 O2 2.215(2) . ?
O4 C6 1.260(3) . ?
N1 C1 1.335(3) . ?
N1 C5 1.337(3) . ?
N3 C7 1.286(3) . ?
N3 N2 1.380(3) . ?
N2 C6 1.350(3) . ?
C1 C2 1.388(3) . ?
C1 C6 1.493(3) . ?
O2 H2 0.8400 . ?
O2 H3S 0.71(4) . ?
N1T C14 1.129(3) . ?
C8 N4 1.359(3) . ?
C8 C9 1.378(3) . ?
C8 C7 1.487(3) . ?
N4 C12 1.332(3) . ?
C12 C11 1.384(4) . ?
C12 H12 0.9500 . ?
C5 C4 1.393(4) . ?
C5 C5 1.486(5) 2 ?
C10 C11 1.376(4) . ?
C10 C9 1.394(4) . ?
C10 H10 0.9500 . ?
C7 C13 1.493(3) . ?
C4 C3 1.385(4) . ?
C4 H4 0.9500 . ?
C9 H9 0.9500 . ?
C2 C3 1.394(4) . ?
C2 H2A 0.9500 . ?
C11 H11 0.9500 . ?
C3 H3 0.9500 . ?
Cl2 O6S 1.419(2) . ?
Cl2 O7S 1.428(2) . ?
Cl2 O8S 1.433(2) . ?
Cl2 O5S 1.442(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.449(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
Cl1S O3SA 1.279(4) . ?
Cl1S O2SB 1.338(5) . ?
Cl1S O1S 1.431(2) . ?
Cl1S O2SA 1.475(4) . ?
Cl1S O4SA 1.497(4) . ?
Cl1S O4SB 1.542(5) . ?
Cl1S O3SB 1.542(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 79.62(12) 2 . ?
N1 Cu1 N2 79.99(8) 2 2 ?
N1 Cu1 N2 158.05(8) . 2 ?
N1 Cu1 N2 158.05(8) 2 . ?
N1 Cu1 N2 80.00(8) . . ?
N2 Cu1 N2 121.24(11) 2 . ?
N3 Cu2 N1T 169.49(9) . . ?
N3 Cu2 N4 80.24(8) . . ?
N1T Cu2 N4 97.10(9) . . ?
N3 Cu2 O4 79.38(7) . . ?
N1T Cu2 O4 101.69(8) . . ?
N4 Cu2 O4 158.47(8) . . ?
N3 Cu2 O2 94.50(8) . . ?
N1T Cu2 O2 95.90(9) . . ?
N4 Cu2 O2 96.40(9) . . ?
O4 Cu2 O2 92.07(8) . . ?
C6 O4 Cu2 109.41(15) . . ?
C1 N1 C5 123.5(2) . . ?
C1 N1 Cu1 117.83(16) . . ?
C5 N1 Cu1 118.31(17) . . ?
C7 N3 N2 123.9(2) . . ?
C7 N3 Cu2 118.16(16) . . ?
N2 N3 Cu2 116.27(14) . . ?
C6 N2 N3 108.92(18) . . ?
C6 N2 Cu1 113.37(16) . . ?
N3 N2 Cu1 134.93(15) . . ?
N1 C1 C2 120.3(2) . . ?
N1 C1 C6 112.0(2) . . ?
C2 C1 C6 127.7(2) . . ?
Cu2 O2 H2 109.5 . . ?
Cu2 O2 H3S 122(4) . . ?
H2 O2 H3S 111.0 . . ?
C14 N1T Cu2 173.7(2) . . ?
O4 C6 N2 125.3(2) . . ?
O4 C6 C1 121.4(2) . . ?
N2 C6 C1 113.3(2) . . ?
N4 C8 C9 121.5(2) . . ?
N4 C8 C7 114.7(2) . . ?
C9 C8 C7 123.7(2) . . ?
C12 N4 C8 119.2(2) . . ?
C12 N4 Cu2 128.52(18) . . ?
C8 N4 Cu2 112.14(16) . . ?
N4 C12 C11 122.3(3) . . ?
N4 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?
N1 C5 C4 119.1(2) . . ?
N1 C5 C5 111.78(14) . 2 ?
C4 C5 C5 129.09(17) . 2 ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
N3 C7 C8 112.0(2) . . ?
N3 C7 C13 126.8(2) . . ?
C8 C7 C13 121.2(2) . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C8 C9 C10 118.8(2) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
C1 C2 C3 117.3(3) . . ?
C1 C2 H2A 121.4 . . ?
C3 C2 H2A 121.4 . . ?
C10 C11 C12 118.9(3) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C4 C3 C2 121.5(2) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
O6S Cl2 O7S 109.51(16) . . ?
O6S Cl2 O8S 110.20(17) . . ?
O7S Cl2 O8S 108.97(16) . . ?
O6S Cl2 O5S 109.67(14) . . ?
O7S Cl2 O5S 109.88(14) . . ?
O8S Cl2 O5S 108.60(14) . . ?
C7 C13 H13A 109.5 . . ?
C7 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C7 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1T C14 C15 179.5(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3SA Cl1S O1S 114.5(3) . . ?
O2SB Cl1S O1S 122.0(3) . . ?
O3SA Cl1S O2SA 115.9(3) . . ?
O1S Cl1S O2SA 105.2(2) . . ?
O3SA Cl1S O4SA 115.6(3) . . ?
O1S Cl1S O4SA 100.86(18) . . ?
O2SA Cl1S O4SA 103.0(3) . . ?
O2SB Cl1S O4SB 108.2(4) . . ?
O1S Cl1S O4SB 111.5(2) . . ?
O2SB Cl1S O3SB 107.2(4) . . ?
O1S Cl1S O3SB 108.1(2) . . ?
O4SB Cl1S O3SB 96.8(3) . . ?

_refine_diff_density_max         0.483
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 1579187'
_audit_update_record             
;
2017-11-11 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H16 Cu3 N12 O14'
_chemical_formula_sum            'C24 H16 Cu3 N12 O14'
_chemical_formula_weight         887.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   15.0153(7)
_cell_length_b                   14.1311(7)
_cell_length_c                   14.3905(7)
_cell_angle_alpha                90
_cell_angle_beta                 98.110(2)
_cell_angle_gamma                90
_cell_volume                     3022.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9813
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      30.53

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.949
_exptl_crystal_F_000             1772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.085
_exptl_absorpt_coefficient_mu    2.185
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5773
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   
;
SADABS 2016/2 Bruker AXS Madison WI USA
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'APEX2 with Photon 100 detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31170
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.883
_diffrn_reflns_theta_max         26.365
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3079
_reflns_number_gt                2742
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0480P)²+9.8405P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3079
_refine_ls_number_parameters     250
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0354
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0903
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.27516(2) 0.55784(2) 0.59513(2) 0.01950(12) Uani 1 1 d . . . . .
Cu2 Cu 0.5000 0.35524(3) 0.7500 0.01995(14) Uani 1 2 d S T P . .
O1 O 0.26599(13) 0.40823(15) 0.58522(13) 0.0235(4) Uani 1 1 d . . . . .
O2 O 0.02998(17) 0.6083(2) 0.4886(2) 0.0567(8) Uani 1 1 d . . . . .
O3 O 0.10530(17) 0.55841(19) 0.62014(17) 0.0391(6) Uani 1 1 d . . . . .
O4 O 0.17492(14) 0.59397(16) 0.50201(14) 0.0264(5) Uani 1 1 d . . . . .
O5 O 0.34967(15) 0.55899(19) 0.47368(16) 0.0380(6) Uani 0.333(8) 1 d D . P A 1
N6 N 0.4230(12) 0.6036(17) 0.4776(11) 0.0287(10) Uani 0.333(8) 1 d D . P A 1
O6 O 0.4735(11) 0.6102(13) 0.5531(11) 0.0457(17) Uani 0.333(8) 1 d D . P A 1
O7 O 0.4517(7) 0.6444(9) 0.4119(6) 0.0455(12) Uani 0.333(8) 1 d D . P A 1
O5A O 0.34967(15) 0.55899(19) 0.47368(16) 0.0380(6) Uani 0.667(8) 1 d D . P A 2
N6A N 0.4275(6) 0.5963(9) 0.4844(6) 0.0287(10) Uani 0.667(8) 1 d D . P A 2
O6A O 0.4537(5) 0.6363(6) 0.5606(5) 0.0457(17) Uani 0.667(8) 1 d D . P A 2
O7A O 0.4712(3) 0.5920(5) 0.4174(3) 0.0455(12) Uani 0.667(8) 1 d D . P A 2
N1 N 0.29796(16) 0.68229(17) 0.66814(16) 0.0208(5) Uani 1 1 d . . . . .
N2 N 0.36496(15) 0.51672(16) 0.69679(16) 0.0180(5) Uani 1 1 d . . . . .
N3 N 0.38909(15) 0.42345(16) 0.70031(16) 0.0186(5) Uani 1 1 d . . . . .
N4 N 0.42587(15) 0.24981(16) 0.70039(16) 0.0193(5) Uani 1 1 d . . . . .
N5 N 0.09942(18) 0.5870(2) 0.53764(19) 0.0302(6) Uani 1 1 d . . . . .
C1 C 0.34827(18) 0.26891(19) 0.64576(18) 0.0184(5) Uani 1 1 d . . . . .
C2 C 0.2943(2) 0.1963(2) 0.60586(19) 0.0230(6) Uani 1 1 d . . . . .
H2 H 0.2382 0.2088 0.5685 0.028 Uiso 1 1 calc R U . . .
C3 C 0.3254(2) 0.1039(2) 0.6224(2) 0.0248(6) Uani 1 1 d . . . . .
H3 H 0.2900 0.0526 0.5951 0.030 Uiso 1 1 calc R U . . .
C4 C 0.4065(2) 0.0853(2) 0.6778(2) 0.0229(6) Uani 1 1 d . . . . .
H4 H 0.4276 0.0223 0.6880 0.028 Uiso 1 1 calc R U . . .
C5 C 0.45610(18) 0.16178(19) 0.71798(19) 0.0193(5) Uani 1 1 d . . . . .
C6 C 0.33083(18) 0.37365(19) 0.63904(19) 0.0191(5) Uani 1 1 d . . . . .
C7 C 0.39695(18) 0.5763(2) 0.75964(19) 0.0194(5) Uani 1 1 d . . . . .
H7 H 0.4389 0.5592 0.8127 0.023 Uiso 1 1 calc R U . . .
C8 C 0.36386(18) 0.6727(2) 0.74343(19) 0.0204(5) Uani 1 1 d . . . . .
C9 C 0.3962(2) 0.7492(2) 0.7983(2) 0.0249(6) Uani 1 1 d . . . . .
H9 H 0.4421 0.7411 0.8503 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3601(2) 0.8384(2) 0.7755(2) 0.0287(7) Uani 1 1 d . . . . .
H10 H 0.3810 0.8922 0.8117 0.034 Uiso 1 1 calc R U . . .
C11 C 0.2936(2) 0.8475(2) 0.6999(2) 0.0286(7) Uani 1 1 d . . . . .
H11 H 0.2682 0.9078 0.6833 0.034 Uiso 1 1 calc R U . . .
C12 C 0.2640(2) 0.7679(2) 0.6478(2) 0.0258(6) Uani 1 1 d . . . . .
H12 H 0.2178 0.7749 0.5958 0.031 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.934(2) . ?
Cu1 O4 1.937(2) . ?
Cu1 N1 2.053(2) . ?
Cu1 O1 2.122(2) . ?
Cu1 O5A 2.204(2) . ?
Cu1 O5 2.204(2) . ?
Cu2 N4 1.935(2) 2_656 ?
Cu2 N4 1.935(2) . ?
Cu2 N3 1.969(2) 2_656 ?
Cu2 N3 1.969(2) . ?
O1 C6 1.255(3) . ?
O2 N5 1.212(4) . ?
O3 N5 1.245(4) . ?
O4 N5 1.312(3) . ?
O5 N6 1.263(13) . ?
N6 O7 1.235(14) . ?
N6 O6 1.238(14) . ?
O5A N6A 1.271(7) . ?
N6A O7A 1.242(8) . ?
N6A O6A 1.247(8) . ?
N1 C12 1.330(4) . ?
N1 C8 1.367(4) . ?
N2 C7 1.279(4) . ?
N2 N3 1.366(3) . ?
N3 C6 1.349(4) . ?
N4 C5 1.336(4) . ?
N4 C1 1.338(4) . ?
C1 C2 1.381(4) . ?
C1 C6 1.504(4) . ?
C2 C3 1.397(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(4) . ?
C4 H4 0.9500 . ?
C5 C5 1.498(5) 2_656 ?
C7 C8 1.457(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(4) . ?
C9 C10 1.392(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 O4 173.37(9) . . ?
N2 Cu1 N1 79.75(9) . . ?
O4 Cu1 N1 100.69(9) . . ?
N2 Cu1 O1 77.48(9) . . ?
O4 Cu1 O1 100.33(9) . . ?
N1 Cu1 O1 153.20(8) . . ?
N2 Cu1 O5A 102.96(9) . . ?
O4 Cu1 O5A 83.18(9) . . ?
N1 Cu1 O5A 109.45(10) . . ?
O1 Cu1 O5A 89.40(9) . . ?
N2 Cu1 O5 102.96(9) . . ?
O4 Cu1 O5 83.18(9) . . ?
N1 Cu1 O5 109.45(10) . . ?
O1 Cu1 O5 89.40(9) . . ?
N4 Cu2 N4 79.30(14) 2_656 . ?
N4 Cu2 N3 80.21(9) 2_656 2_656 ?
N4 Cu2 N3 157.50(10) . 2_656 ?
N4 Cu2 N3 157.50(10) 2_656 . ?
N4 Cu2 N3 80.21(9) . . ?
N3 Cu2 N3 121.39(14) 2_656 . ?
C6 O1 Cu1 108.01(17) . . ?
N5 O4 Cu1 109.85(17) . . ?
N6 O5 Cu1 120.4(8) . . ?
O7 N6 O6 113.6(14) . . ?
O7 N6 O5 126.5(15) . . ?
O6 N6 O5 119.9(15) . . ?
N6A O5A Cu1 117.9(4) . . ?
O7A N6A O6A 124.7(7) . . ?
O7A N6A O5A 117.5(7) . . ?
O6A N6A O5A 117.8(7) . . ?
C12 N1 C8 118.5(3) . . ?
C12 N1 Cu1 129.5(2) . . ?
C8 N1 Cu1 111.73(18) . . ?
C7 N2 N3 122.6(2) . . ?
C7 N2 Cu1 119.29(19) . . ?
N3 N2 Cu1 118.09(17) . . ?
C6 N3 N2 109.6(2) . . ?
C6 N3 Cu2 114.78(18) . . ?
N2 N3 Cu2 133.79(18) . . ?
C5 N4 C1 122.9(2) . . ?
C5 N4 Cu2 118.99(18) . . ?
C1 N4 Cu2 117.99(18) . . ?
O2 N5 O3 125.1(3) . . ?
O2 N5 O4 118.3(3) . . ?
O3 N5 O4 116.6(3) . . ?
N4 C1 C2 120.4(3) . . ?
N4 C1 C6 111.5(2) . . ?
C2 C1 C6 128.2(3) . . ?
C1 C2 C3 117.5(3) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C4 C3 C2 121.5(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 117.9(3) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N4 C5 C4 119.8(3) . . ?
N4 C5 C5 111.25(15) . 2_656 ?
C4 C5 C5 128.97(17) . 2_656 ?
O1 C6 N3 125.1(3) . . ?
O1 C6 C1 122.4(2) . . ?
N3 C6 C1 112.4(2) . . ?
N2 C7 C8 114.6(2) . . ?
N2 C7 H7 122.7 . . ?
C8 C7 H7 122.7 . . ?
N1 C8 C9 122.0(3) . . ?
N1 C8 C7 114.4(2) . . ?
C9 C8 C7 123.6(3) . . ?
C8 C9 C10 118.5(3) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
C9 C10 H10 120.4 . . ?
C10 C11 C12 119.5(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
N1 C12 C11 122.3(3) . . ?
N1 C12 H12 118.9 . . ?
C11 C12 H12 118.9 . . ?

_refine_diff_density_max         0.756
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.098

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 1579188'
_audit_update_record             
;
2017-11-11 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_complex4            
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: This was a weakly diffracting crystal and measured to ca. 50 deg/2theta.
Despite the shortage of high angle data the data:parameter ratio was greater than 10:1 which was adequate for refinement purposes.
 
;
_vrf_PLAT232_complex4            
;
PROBLEM: Hirshfeld Test Diff (M-X)  Mn1    --  O3      ..        7.2 s.u.  
RESPONSE: Acknowledged but no particularly problematic evidence for atom mis-asignment or disorder in this part of the structure.

;
_vrf_PLAT341_complex4            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00614 Ang.  
RESPONSE: ...
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C26 H28 Cl4 Mn3 N10 O5, 0.33 (C H4 O), 0.67 (H2 O)'
_chemical_formula_sum            'C26.33 H30.66 Cl4 Mn3 N10 O6'
_chemical_formula_weight         889.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3696(5)
_cell_length_b                   12.7637(6)
_cell_length_c                   14.6867(6)
_cell_angle_alpha                75.3919(17)
_cell_angle_beta                 70.8407(17)
_cell_angle_gamma                75.991(2)
_cell_volume                     1749.63(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9882
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      24.67

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_F_000             899
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.427
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6533
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   
;
SADABS 2016/2, Bruker AXS, Madison WI USA
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26967
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.914
_diffrn_reflns_theta_max         24.693
_diffrn_reflns_theta_full        24.693
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5930
_reflns_number_gt                4944
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Chloride disoredred over two sites and lattice solvent modelled as 
disordered H2O/MeOH combination; 1/3 methanol and 2/3 water.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0444P)²+5.0777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5930
_refine_ls_number_parameters     480
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1173
_refine_ls_wR_factor_gt          0.1059
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.97510(5) 0.37248(4) 0.26679(4) 0.01755(15) Uani 1 1 d . . . . .
Mn2 Mn 1.12421(6) 0.17335(5) 0.05518(4) 0.02763(17) Uani 1 1 d . . . . .
Mn3 Mn 0.63609(6) 0.25063(5) 0.45530(4) 0.02447(16) Uani 1 1 d D . . . .
Cl1 Cl 1.01580(12) 0.04242(9) 0.18570(9) 0.0429(3) Uani 1 1 d . . . . .
Cl2 Cl 0.99040(11) 0.27638(9) -0.05346(8) 0.0344(2) Uani 1 1 d . . . . .
Cl5 Cl 0.53661(11) 0.29323(10) 0.32239(8) 0.0355(3) Uani 1 1 d . . . . .
Cl6A Cl 0.8075(3) 0.0914(2) 0.4803(3) 0.0325(7) Uani 0.633(7) 1 d D . P A 1
Cl6B Cl 0.8017(6) 0.0874(5) 0.4447(4) 0.0325(7) Uani 0.367(7) 1 d D . P A 2
O1 O 1.1379(2) 0.2945(2) 0.13571(17) 0.0201(5) Uani 1 1 d . . . . .
O2 O 0.7798(3) 0.3694(2) 0.39969(18) 0.0217(6) Uani 1 1 d . . . . .
O3 O 0.8756(3) 0.5146(2) 0.1656(2) 0.0240(6) Uani 1 1 d D . . . .
H3 H 0.917(4) 0.563(3) 0.146(3) 0.029 Uiso 1 1 d D U . . .
C25 C 0.8221(6) 0.4975(4) 0.0963(4) 0.0466(12) Uani 1 1 d . . . . .
H25A H 0.8968 0.4610 0.0474 0.070 Uiso 1 1 calc R U . . .
H25B H 0.7807 0.5683 0.0636 0.070 Uiso 1 1 calc R U . . .
H25C H 0.7510 0.4510 0.1289 0.070 Uiso 1 1 calc R U . . .
O4 O 1.0545(3) 0.2265(2) 0.36317(19) 0.0246(6) Uani 1 1 d D . . . .
H4 H 0.997(4) 0.186(3) 0.392(3) 0.030 Uiso 1 1 d D U . . .
C26 C 1.1927(5) 0.1664(4) 0.3424(3) 0.0354(10) Uani 1 1 d . . . . .
H26A H 1.2114 0.1317 0.2859 0.053 Uiso 1 1 calc R U . . .
H26B H 1.2036 0.1096 0.3996 0.053 Uiso 1 1 calc R U . . .
H26C H 1.2581 0.2167 0.3273 0.053 Uiso 1 1 calc R U . . .
O6 O 0.8596(3) 0.2719(2) 0.2305(2) 0.0285(6) Uani 1 1 d D . . . .
H6A H 0.888(5) 0.2055(18) 0.229(3) 0.034 Uiso 1 1 d D U . . .
H6B H 0.775(2) 0.279(4) 0.244(3) 0.034 Uiso 1 1 d D U . . .
C1 C 1.2220(5) -0.0434(4) -0.0517(3) 0.0376(10) Uani 1 1 d . . . . .
H1 H 1.1306 -0.0568 -0.0177 0.045 Uiso 1 1 calc R U . . .
C2 C 1.3081(5) -0.1139(4) -0.1131(4) 0.0398(11) Uani 1 1 d . . . . .
H2 H 1.2773 -0.1752 -0.1197 0.048 Uiso 1 1 calc R U . . .
C3 C 1.4391(5) -0.0931(4) -0.1643(3) 0.0393(11) Uani 1 1 d . . . . .
H3A H 1.4994 -0.1382 -0.2091 0.047 Uiso 1 1 calc R U . . .
C4 C 1.4825(4) -0.0053(4) -0.1499(3) 0.0333(10) Uani 1 1 d . . . . .
H4A H 1.5735 0.0095 -0.1834 0.040 Uiso 1 1 calc R U . . .
C5 C 1.3909(4) 0.0599(3) -0.0860(3) 0.0253(8) Uani 1 1 d . . . . .
C6 C 1.4271(4) 0.1523(3) -0.0600(3) 0.0254(8) Uani 1 1 d . . . . .
C7 C 1.2596(4) 0.3219(3) 0.1032(2) 0.0189(7) Uani 1 1 d . . . . .
C8 C 1.2816(4) 0.4102(3) 0.1431(2) 0.0190(7) Uani 1 1 d . . . . .
C9 C 1.4063(4) 0.4486(3) 0.1138(3) 0.0235(8) Uani 1 1 d . . . . .
H9 H 1.4848 0.4165 0.0679 0.028 Uiso 1 1 calc R U . . .
C10 C 1.4140(4) 0.5337(3) 0.1523(3) 0.0283(9) Uani 1 1 d . . . . .
H10 H 1.4976 0.5624 0.1317 0.034 Uiso 1 1 calc R U . . .
C11 C 1.2992(4) 0.5779(3) 0.2213(3) 0.0257(8) Uani 1 1 d . . . . .
H11 H 1.3024 0.6372 0.2482 0.031 Uiso 1 1 calc R U . . .
C12 C 1.1800(4) 0.5326(3) 0.2497(3) 0.0202(8) Uani 1 1 d . . . . .
C13 C 1.0539(4) 0.5670(3) 0.3283(3) 0.0195(7) Uani 1 1 d . . . . .
C14 C 1.0385(4) 0.6535(3) 0.3743(3) 0.0251(8) Uani 1 1 d . . . . .
H14 H 1.1064 0.6996 0.3527 0.030 Uiso 1 1 calc R U . . .
C15 C 0.9222(4) 0.6711(3) 0.4524(3) 0.0268(9) Uani 1 1 d . . . . .
H15 H 0.9089 0.7304 0.4846 0.032 Uiso 1 1 calc R U . . .
C16 C 0.8251(4) 0.6024(3) 0.4836(3) 0.0233(8) Uani 1 1 d . . . . .
H16 H 0.7460 0.6122 0.5383 0.028 Uiso 1 1 calc R U . . .
C17 C 0.8469(4) 0.5185(3) 0.4325(2) 0.0190(7) Uani 1 1 d . . . . .
C18 C 0.7533(4) 0.4374(3) 0.4593(3) 0.0189(7) Uani 1 1 d . . . . .
C19 C 0.4704(4) 0.3541(3) 0.6325(3) 0.0209(8) Uani 1 1 d . . . . .
C20 C 0.3939(4) 0.2627(3) 0.6485(3) 0.0214(8) Uani 1 1 d . . . . .
C21 C 0.2799(4) 0.2433(3) 0.7274(3) 0.0255(8) Uani 1 1 d . . . . .
H21 H 0.2474 0.2874 0.7764 0.031 Uiso 1 1 calc R U . . .
C22 C 0.2136(4) 0.1584(3) 0.7341(3) 0.0305(9) Uani 1 1 d . . . . .
H22 H 0.1348 0.1436 0.7877 0.037 Uiso 1 1 calc R U . . .
C23 C 0.2634(5) 0.0958(4) 0.6621(3) 0.0353(10) Uani 1 1 d . . . . .
H23 H 0.2193 0.0375 0.6649 0.042 Uiso 1 1 calc R U . . .
C24 C 0.3786(5) 0.1195(3) 0.5857(3) 0.0348(10) Uani 1 1 d . . . . .
H24 H 0.4126 0.0760 0.5362 0.042 Uiso 1 1 calc R U . . .
N1 N 1.2602(3) 0.0422(3) -0.0377(2) 0.0292(8) Uani 1 1 d . . . . .
N2 N 1.3321(3) 0.1990(3) 0.0069(2) 0.0232(7) Uani 1 1 d . . . . .
N3 N 1.3660(3) 0.2821(3) 0.0370(2) 0.0213(7) Uani 1 1 d . . . . .
N4 N 1.1708(3) 0.4508(2) 0.2109(2) 0.0185(6) Uani 1 1 d . . . . .
N5 N 0.9579(3) 0.5024(2) 0.3555(2) 0.0175(6) Uani 1 1 d . . . . .
N6 N 0.6544(3) 0.4399(3) 0.5417(2) 0.0215(7) Uani 1 1 d . . . . .
N7 N 0.5822(3) 0.3549(2) 0.5589(2) 0.0206(7) Uani 1 1 d . . . . .
N8 N 0.4450(3) 0.2006(3) 0.5778(2) 0.0265(7) Uani 1 1 d . . . . .
N9 N 0.4231(3) 0.4274(3) 0.6918(2) 0.0243(7) Uani 1 1 d . . . . .
H9A H 0.4685 0.4811 0.6822 0.029 Uiso 1 1 calc R U . . .
H9B H 0.3466 0.4221 0.7404 0.029 Uiso 1 1 calc R U . . .
N10 N 1.5527(4) 0.1803(3) -0.1018(3) 0.0372(9) Uani 1 1 d . . . . .
H10A H 1.5741 0.2333 -0.0839 0.045 Uiso 1 1 calc R U . . .
H10B H 1.6138 0.1459 -0.1471 0.045 Uiso 1 1 calc R U . . .
O0AA O 1.7618(6) 0.1305(5) -0.2910(5) 0.0395(13) Uani 0.67 1 d . . P B 1
H0AD H 1.7258 0.1191 -0.3327 0.059 Uiso 0.67 1 d R U P B 1
H0AE H 1.8175 0.0693 -0.2784 0.059 Uiso 0.67 1 d R U P B 1
O1AA O 1.7870(12) 0.1377(10) -0.2489(9) 0.041(3) Uani 0.33 1 d . . P C 2
H1AA H 1.8424 0.0877 -0.2247 0.062 Uiso 0.33 1 d R U P C 2
C0AA C 1.8018(17) 0.1211(12) -0.3470(13) 0.035(3) Uani 0.33 1 d . . P C 2
H0AA H 1.7884 0.1926 -0.3902 0.052 Uiso 0.33 1 calc R U P C 2
H0AB H 1.7322 0.0789 -0.3432 0.052 Uiso 0.33 1 calc R U P C 2
H0AC H 1.8948 0.0806 -0.3732 0.052 Uiso 0.33 1 calc R U P C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O4 2.201(3) . ?
Mn1 O6 2.208(3) . ?
Mn1 N4 2.295(3) . ?
Mn1 N5 2.297(3) . ?
Mn1 O3 2.303(3) . ?
Mn1 O2 2.306(2) . ?
Mn1 O1 2.359(2) . ?
Mn2 N2 2.116(3) . ?
Mn2 O1 2.225(2) . ?
Mn2 N1 2.323(3) . ?
Mn2 Cl1 2.3686(12) . ?
Mn2 Cl2 2.3900(12) . ?
Mn3 N7 2.121(3) . ?
Mn3 O2 2.204(3) . ?
Mn3 N8 2.294(3) . ?
Mn3 Cl6B 2.360(5) . ?
Mn3 Cl5 2.3844(12) . ?
Mn3 Cl6A 2.393(3) . ?
O1 C7 1.295(4) . ?
O2 C18 1.305(4) . ?
O3 C25 1.391(5) . ?
O3 H3 0.782(19) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O4 C26 1.426(5) . ?
O4 H4 0.816(19) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
O6 H6A 0.831(19) . ?
O6 H6B 0.818(19) . ?
C1 N1 1.331(5) . ?
C1 C2 1.382(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.373(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.380(6) . ?
C4 H4A 0.9500 . ?
C5 N1 1.351(5) . ?
C5 C6 1.487(6) . ?
C6 N2 1.292(5) . ?
C6 N10 1.338(5) . ?
C7 N3 1.302(5) . ?
C7 C8 1.487(5) . ?
C8 N4 1.342(5) . ?
C8 C9 1.390(5) . ?
C9 C10 1.374(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.386(5) . ?
C11 H11 0.9500 . ?
C12 N4 1.344(5) . ?
C12 C13 1.490(5) . ?
C13 N5 1.341(5) . ?
C13 C14 1.386(5) . ?
C14 C15 1.383(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(5) . ?
C16 H16 0.9500 . ?
C17 N5 1.340(5) . ?
C17 C18 1.483(5) . ?
C18 N6 1.307(5) . ?
C19 N7 1.300(5) . ?
C19 N9 1.336(5) . ?
C19 C20 1.494(5) . ?
C20 N8 1.356(5) . ?
C20 C21 1.378(5) . ?
C21 C22 1.386(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.375(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(6) . ?
C23 H23 0.9500 . ?
C24 N8 1.337(5) . ?
C24 H24 0.9500 . ?
N2 N3 1.402(4) . ?
N6 N7 1.391(4) . ?
N9 H9A 0.8800 . ?
N9 H9B 0.8800 . ?
N10 H10A 0.8800 . ?
N10 H10B 0.8800 . ?
O0AA H0AD 0.8700 . ?
O0AA H0AE 0.8699 . ?
O1AA C0AA 1.461(17) . ?
O1AA H1AA 0.8400 . ?
C0AA H0AA 0.9800 . ?
C0AA H0AB 0.9800 . ?
C0AA H0AC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Mn1 O6 89.67(11) . . ?
O4 Mn1 N4 96.91(10) . . ?
O6 Mn1 N4 143.99(11) . . ?
O4 Mn1 N5 98.33(10) . . ?
O6 Mn1 N5 145.14(11) . . ?
N4 Mn1 N5 68.87(10) . . ?
O4 Mn1 O3 173.93(10) . . ?
O6 Mn1 O3 84.41(10) . . ?
N4 Mn1 O3 88.69(10) . . ?
N5 Mn1 O3 85.84(10) . . ?
O4 Mn1 O2 81.74(10) . . ?
O6 Mn1 O2 78.23(10) . . ?
N4 Mn1 O2 137.71(10) . . ?
N5 Mn1 O2 69.54(9) . . ?
O3 Mn1 O2 95.70(9) . . ?
O4 Mn1 O1 85.88(9) . . ?
O6 Mn1 O1 75.97(9) . . ?
N4 Mn1 O1 69.29(9) . . ?
N5 Mn1 O1 138.16(10) . . ?
O3 Mn1 O1 93.96(9) . . ?
O2 Mn1 O1 151.37(9) . . ?
N2 Mn2 O1 72.50(10) . . ?
N2 Mn2 N1 71.10(12) . . ?
O1 Mn2 N1 142.10(11) . . ?
N2 Mn2 Cl1 129.92(10) . . ?
O1 Mn2 Cl1 101.53(7) . . ?
N1 Mn2 Cl1 93.77(9) . . ?
N2 Mn2 Cl2 113.60(9) . . ?
O1 Mn2 Cl2 104.91(7) . . ?
N1 Mn2 Cl2 98.99(9) . . ?
Cl1 Mn2 Cl2 115.85(5) . . ?
N7 Mn3 O2 72.34(10) . . ?
N7 Mn3 N8 72.27(12) . . ?
O2 Mn3 N8 144.52(11) . . ?
N7 Mn3 Cl6B 128.27(18) . . ?
O2 Mn3 Cl6B 98.40(16) . . ?
N8 Mn3 Cl6B 105.26(16) . . ?
N7 Mn3 Cl5 121.97(9) . . ?
O2 Mn3 Cl5 99.17(7) . . ?
N8 Mn3 Cl5 97.29(9) . . ?
Cl6B Mn3 Cl5 109.69(15) . . ?
N7 Mn3 Cl6A 114.80(14) . . ?
O2 Mn3 Cl6A 96.00(10) . . ?
N8 Mn3 Cl6A 100.87(11) . . ?
Cl5 Mn3 Cl6A 123.21(11) . . ?
C7 O1 Mn2 110.8(2) . . ?
C7 O1 Mn1 117.9(2) . . ?
Mn2 O1 Mn1 131.25(11) . . ?
C18 O2 Mn3 111.6(2) . . ?
C18 O2 Mn1 119.2(2) . . ?
Mn3 O2 Mn1 128.69(11) . . ?
C25 O3 Mn1 122.7(3) . . ?
C25 O3 H3 113(3) . . ?
Mn1 O3 H3 112(3) . . ?
O3 C25 H25A 109.5 . . ?
O3 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O3 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 O4 Mn1 125.7(2) . . ?
C26 O4 H4 112(3) . . ?
Mn1 O4 H4 113(3) . . ?
O4 C26 H26A 109.5 . . ?
O4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Mn1 O6 H6A 122(3) . . ?
Mn1 O6 H6B 126(3) . . ?
H6A O6 H6B 105(5) . . ?
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.4(4) . . ?
C3 C2 H2 120.8 . . ?
C1 C2 H2 120.8 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4A 120.7 . . ?
C3 C4 H4A 120.7 . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 C6 113.6(3) . . ?
C4 C5 C6 123.8(4) . . ?
N2 C6 N10 123.5(4) . . ?
N2 C6 C5 115.5(3) . . ?
N10 C6 C5 120.9(4) . . ?
O1 C7 N3 127.1(3) . . ?
O1 C7 C8 117.5(3) . . ?
N3 C7 C8 115.3(3) . . ?
N4 C8 C9 121.8(3) . . ?
N4 C8 C7 114.7(3) . . ?
C9 C8 C7 123.5(3) . . ?
C10 C9 C8 118.9(4) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C9 C10 C11 119.9(3) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C12 C11 C10 118.0(4) . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 121.0 . . ?
N4 C12 C11 122.4(3) . . ?
N4 C12 C13 114.4(3) . . ?
C11 C12 C13 123.1(3) . . ?
N5 C13 C14 122.0(3) . . ?
N5 C13 C12 114.0(3) . . ?
C14 C13 C12 123.9(3) . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C16 C15 C14 120.0(3) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 118.0(3) . . ?
C15 C16 H16 121.0 . . ?
C17 C16 H16 121.0 . . ?
N5 C17 C16 122.2(3) . . ?
N5 C17 C18 114.0(3) . . ?
C16 C17 C18 123.8(3) . . ?
O2 C18 N6 126.8(3) . . ?
O2 C18 C17 117.0(3) . . ?
N6 C18 C17 116.2(3) . . ?
N7 C19 N9 124.7(4) . . ?
N7 C19 C20 115.1(3) . . ?
N9 C19 C20 120.2(3) . . ?
N8 C20 C21 122.4(4) . . ?
N8 C20 C19 114.3(3) . . ?
C21 C20 C19 123.3(3) . . ?
C20 C21 C22 118.9(4) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C23 C22 C21 119.2(4) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 118.6(4) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
N8 C24 C23 123.4(4) . . ?
N8 C24 H24 118.3 . . ?
C23 C24 H24 118.3 . . ?
C1 N1 C5 117.6(4) . . ?
C1 N1 Mn2 127.5(3) . . ?
C5 N1 Mn2 114.8(3) . . ?
C6 N2 N3 116.9(3) . . ?
C6 N2 Mn2 123.1(3) . . ?
N3 N2 Mn2 119.3(2) . . ?
C7 N3 N2 109.5(3) . . ?
C8 N4 C12 119.0(3) . . ?
C8 N4 Mn1 120.0(2) . . ?
C12 N4 Mn1 120.9(2) . . ?
C17 N5 C13 119.2(3) . . ?
C17 N5 Mn1 119.8(2) . . ?
C13 N5 Mn1 120.9(2) . . ?
C18 N6 N7 108.9(3) . . ?
C19 N7 N6 116.2(3) . . ?
C19 N7 Mn3 122.7(3) . . ?
N6 N7 Mn3 120.3(2) . . ?
C24 N8 C20 117.4(3) . . ?
C24 N8 Mn3 127.5(3) . . ?
C20 N8 Mn3 115.1(2) . . ?
C19 N9 H9A 120.0 . . ?
C19 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
C6 N10 H10A 120.0 . . ?
C6 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
H0AD O0AA H0AE 104.5 . . ?
C0AA O1AA H1AA 108.2 . . ?
O1AA C0AA H0AA 109.5 . . ?
O1AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
O1AA C0AA H0AC 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?

_refine_diff_density_max         0.644
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.094

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 1579186'
_audit_update_record             
;
2017-11-11 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT341_complex2            
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00625 Ang.  
RESPONSE: Very small crystal 0.10 x 0.04 x 0.02 mm. Data collected to 
52 deg/2theta.
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H20 Cl4 Cu3 N8 O2'
_chemical_formula_sum            'C26 H20 Cl4 Cu3 N8 O2'
_chemical_formula_weight         808.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   13.099(3)
_cell_length_b                   13.734(3)
_cell_length_c                   15.973(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.33(3)
_cell_angle_gamma                90
_cell_volume                     2757.6(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3260
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      26.15

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_F_000             1612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.725
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5965
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6314
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.077
_diffrn_reflns_theta_max         26.375
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             2767
_reflns_number_gt                2185
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Structure initially solved in cc, at later stages of refinement ADDSYM 
within PLATON identified a higher symmetry I2/a space group and refinement
completed in this monoclinic space group.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0560P)²+21.1780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2767
_refine_ls_number_parameters     196
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1162
_refine_ls_wR_factor_gt          0.1009
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.2500 1.09339(5) 0.0000 0.02051(19) Uani 1 2 d S T P . .
Cu2 Cu 0.11438(4) 0.91450(3) 0.21444(3) 0.02256(17) Uani 1 1 d . . . . .
Cl1 Cl 0.08716(8) 1.08654(8) -0.15061(7) 0.0273(2) Uani 1 1 d . . . . .
Cl2 Cl 0.13782(10) 0.89905(8) 0.35743(7) 0.0326(3) Uani 1 1 d . . . . .
O1 O 0.1274(2) 1.0587(2) 0.20835(18) 0.0228(6) Uani 1 1 d . . . . .
N1 N 0.2033(3) 1.2054(2) 0.0576(2) 0.0171(6) Uani 1 1 d . . . . .
N2 N 0.1624(3) 1.0231(2) 0.0773(2) 0.0172(7) Uani 1 1 d . . . . .
N3 N 0.1435(3) 0.9291(2) 0.1009(2) 0.0199(7) Uani 1 1 d . . . . .
N4 N 0.1109(3) 0.7751(2) 0.1791(2) 0.0227(7) Uani 1 1 d . . . . .
C1 C 0.2258(3) 1.2967(3) 0.0364(3) 0.0181(8) Uani 1 1 d . . . . .
C2 C 0.2057(3) 1.3759(3) 0.0833(3) 0.0228(8) Uani 1 1 d . . . . .
H2 H 0.2212 1.4388 0.0694 0.027 Uiso 1 1 calc R U . . .
C3 C 0.1618(4) 1.3591(3) 0.1515(3) 0.0258(9) Uani 1 1 d . . . . .
H3 H 0.1465 1.4113 0.1829 0.031 Uiso 1 1 calc R U . . .
C4 C 0.1406(3) 1.2648(3) 0.1731(3) 0.0219(8) Uani 1 1 d . . . . .
H4 H 0.1118 1.2530 0.2191 0.026 Uiso 1 1 calc R U . . .
C5 C 0.1636(3) 1.1888(3) 0.1242(3) 0.0189(8) Uani 1 1 d . . . . .
C6 C 0.1506(3) 1.0832(3) 0.1405(3) 0.0188(8) Uani 1 1 d . . . . .
C7 C 0.1266(3) 0.8550(3) 0.0498(3) 0.0202(8) Uani 1 1 d . . . . .
C8 C 0.1212(4) 0.8548(3) -0.0445(3) 0.0270(9) Uani 1 1 d . . . . .
H8A H 0.0495 0.8418 -0.0784 0.040 Uiso 1 1 calc R U . . .
H8B H 0.1676 0.8054 -0.0555 0.040 Uiso 1 1 calc R U . . .
H8C H 0.1429 0.9173 -0.0604 0.040 Uiso 1 1 calc R U . . .
C9 C 0.1043(3) 0.7644(3) 0.0929(3) 0.0213(8) Uani 1 1 d . . . . .
C10 C 0.0746(4) 0.6775(3) 0.0500(3) 0.0300(10) Uani 1 1 d . . . . .
H10 H 0.0714 0.6710 -0.0087 0.036 Uiso 1 1 calc R U . . .
C11 C 0.0493(4) 0.5994(3) 0.0961(3) 0.0358(11) Uani 1 1 d . . . . .
H11 H 0.0267 0.5406 0.0681 0.043 Uiso 1 1 calc R U . . .
C12 C 0.0582(4) 0.6101(3) 0.1838(3) 0.0342(11) Uani 1 1 d . . . . .
H12 H 0.0433 0.5582 0.2159 0.041 Uiso 1 1 calc R U . . .
C13 C 0.0894(4) 0.6987(3) 0.2229(3) 0.0291(10) Uani 1 1 d . . . . .
H13 H 0.0957 0.7055 0.2821 0.035 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N1 1.975(3) . ?
Cu1 N1 1.975(3) 2 ?
Cu1 N2 2.138(3) . ?
Cu1 N2 2.138(3) 2 ?
Cu1 Cl1 2.7314(16) 2 ?
Cu1 Cl1 2.7314(16) . ?
Cu2 N3 1.966(3) . ?
Cu2 O1 1.992(3) . ?
Cu2 N4 1.993(3) . ?
Cu2 Cl2 2.2273(15) . ?
Cu2 Cl1 2.5488(14) 5_575 ?
Cl1 Cu2 2.5488(14) 5_575 ?
O1 C6 1.251(5) . ?
N1 C5 1.330(5) . ?
N1 C1 1.352(5) . ?
N2 C6 1.346(5) . ?
N2 N3 1.387(4) . ?
N3 C7 1.284(5) . ?
N4 C13 1.334(5) . ?
N4 C9 1.364(5) . ?
C1 C2 1.387(5) . ?
C1 C1 1.475(8) 2 ?
C2 C3 1.385(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.388(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.387(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.492(5) . ?
C7 C8 1.487(6) . ?
C7 C9 1.490(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.377(6) . ?
C10 C11 1.393(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(7) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cu1 N1 77.71(19) . 2 ?
N1 Cu1 N2 78.22(12) . . ?
N1 Cu1 N2 155.12(13) 2 . ?
N1 Cu1 N2 155.12(13) . 2 ?
N1 Cu1 N2 78.22(12) 2 2 ?
N2 Cu1 N2 126.33(17) . 2 ?
N1 Cu1 Cl1 83.34(10) . 2 ?
N1 Cu1 Cl1 99.77(10) 2 2 ?
N2 Cu1 Cl1 83.59(10) . 2 ?
N2 Cu1 Cl1 94.62(10) 2 2 ?
N1 Cu1 Cl1 99.76(10) . . ?
N1 Cu1 Cl1 83.34(10) 2 . ?
N2 Cu1 Cl1 94.62(10) . . ?
N2 Cu1 Cl1 83.59(10) 2 . ?
Cl1 Cu1 Cl1 176.05(5) 2 . ?
N3 Cu2 O1 79.18(12) . . ?
N3 Cu2 N4 80.29(14) . . ?
O1 Cu2 N4 159.46(13) . . ?
N3 Cu2 Cl2 161.65(11) . . ?
O1 Cu2 Cl2 98.96(9) . . ?
N4 Cu2 Cl2 100.64(11) . . ?
N3 Cu2 Cl1 94.56(11) . 5_575 ?
O1 Cu2 Cl1 94.55(9) . 5_575 ?
N4 Cu2 Cl1 86.72(11) . 5_575 ?
Cl2 Cu2 Cl1 103.78(5) . 5_575 ?
Cu2 Cl1 Cu1 144.79(5) 5_575 . ?
C6 O1 Cu2 110.8(3) . . ?
C5 N1 C1 121.4(3) . . ?
C5 N1 Cu1 118.8(3) . . ?
C1 N1 Cu1 119.2(3) . . ?
C6 N2 N3 107.5(3) . . ?
C6 N2 Cu1 110.5(2) . . ?
N3 N2 Cu1 138.0(2) . . ?
C7 N3 N2 125.3(3) . . ?
C7 N3 Cu2 117.5(3) . . ?
N2 N3 Cu2 116.1(2) . . ?
C13 N4 C9 118.8(4) . . ?
C13 N4 Cu2 126.7(3) . . ?
C9 N4 Cu2 112.3(3) . . ?
N1 C1 C2 120.3(3) . . ?
N1 C1 C1 111.7(2) . 2 ?
C2 C1 C1 128.0(2) . 2 ?
C3 C2 C1 118.5(4) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 120.5(4) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 118.1(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 121.2(4) . . ?
N1 C5 C6 113.3(3) . . ?
C4 C5 C6 125.5(4) . . ?
O1 C6 N2 126.3(4) . . ?
O1 C6 C5 118.7(3) . . ?
N2 C6 C5 115.0(3) . . ?
N3 C7 C8 126.5(4) . . ?
N3 C7 C9 112.9(3) . . ?
C8 C7 C9 120.4(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N4 C9 C10 121.7(4) . . ?
N4 C9 C7 114.3(3) . . ?
C10 C9 C7 124.0(4) . . ?
C9 C10 C11 118.7(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 119.4(4) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C13 C12 C11 119.0(4) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
N4 C13 C12 122.5(4) . . ?
N4 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 N3 C7 165.3(4) . . . . ?
Cu1 N2 N3 C7 -40.7(6) . . . . ?
C6 N2 N3 Cu2 -2.8(4) . . . . ?
Cu1 N2 N3 Cu2 151.2(2) . . . . ?
C5 N1 C1 C2 -1.2(6) . . . . ?
Cu1 N1 C1 C2 -172.0(3) . . . . ?
C5 N1 C1 C1 177.0(4) . . . 2 ?
Cu1 N1 C1 C1 6.1(5) . . . 2 ?
N1 C1 C2 C3 -0.4(6) . . . . ?
C1 C1 C2 C3 -178.2(5) 2 . . . ?
C1 C2 C3 C4 1.2(7) . . . . ?
C2 C3 C4 C5 -0.6(6) . . . . ?
C1 N1 C5 C4 1.9(6) . . . . ?
Cu1 N1 C5 C4 172.8(3) . . . . ?
C1 N1 C5 C6 -176.4(3) . . . . ?
Cu1 N1 C5 C6 -5.6(5) . . . . ?
C3 C4 C5 N1 -1.0(6) . . . . ?
C3 C4 C5 C6 177.1(4) . . . . ?
Cu2 O1 C6 N2 2.0(5) . . . . ?
Cu2 O1 C6 C5 179.9(3) . . . . ?
N3 N2 C6 O1 0.4(5) . . . . ?
Cu1 N2 C6 O1 -161.3(3) . . . . ?
N3 N2 C6 C5 -177.5(3) . . . . ?
Cu1 N2 C6 C5 20.8(4) . . . . ?
N1 C5 C6 O1 170.6(4) . . . . ?
C4 C5 C6 O1 -7.7(6) . . . . ?
N1 C5 C6 N2 -11.3(5) . . . . ?
C4 C5 C6 N2 170.4(4) . . . . ?
N2 N3 C7 C8 -1.6(7) . . . . ?
Cu2 N3 C7 C8 166.3(3) . . . . ?
N2 N3 C7 C9 -177.6(3) . . . . ?
Cu2 N3 C7 C9 -9.7(5) . . . . ?
C13 N4 C9 C10 1.0(6) . . . . ?
Cu2 N4 C9 C10 -163.5(4) . . . . ?
C13 N4 C9 C7 178.2(4) . . . . ?
Cu2 N4 C9 C7 13.6(4) . . . . ?
N3 C7 C9 N4 -3.0(5) . . . . ?
C8 C7 C9 N4 -179.3(4) . . . . ?
N3 C7 C9 C10 174.1(4) . . . . ?
C8 C7 C9 C10 -2.2(6) . . . . ?
N4 C9 C10 C11 0.9(7) . . . . ?
C7 C9 C10 C11 -176.0(4) . . . . ?
C9 C10 C11 C12 -2.1(8) . . . . ?
C10 C11 C12 C13 1.5(8) . . . . ?
C9 N4 C13 C12 -1.7(7) . . . . ?
Cu2 N4 C13 C12 160.4(4) . . . . ?
C11 C12 C13 N4 0.4(8) . . . . ?

_refine_diff_density_max         0.853
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.109

_shelxl_version_number           2013-3

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_complex5
_database_code_depnum_ccdc_archive 'CCDC 1579189'
_audit_update_record             
;
2017-12-06 deposited with the CCDC.
2017-12-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_complex5            
;
PROBLEM: D-H Without Acceptor      O9       --H9B       .     Please Check 
RESPONSE: O9-H9B is oriented into a lattice void associated with a poorly
          defined Et2O molecule which was disordered over at least two 
          positions. Residual electron density in this region +1.7e A-3
          indicated further unresolved disorder. The instability in the
          refinement of this ether solvate led to eventual treatment with
          SQUEEZE and a smoother convergence of the remaining solvent and
          anion molecules.     
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C52 H52 Fe4 N16 O10, 6 (C F3 S O3), 1.5(C2 H3 N), C4H10O
;
_chemical_formula_sum            'C65 H66.50 F18 Fe4 N17.50 O29 S6'
_chemical_formula_weight         2314.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.2861(10)
_cell_length_b                   18.7512(11)
_cell_length_c                   19.8454(12)
_cell_angle_alpha                79.965(2)
_cell_angle_beta                 76.015(2)
_cell_angle_gamma                68.805(2)
_cell_volume                     5122.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9600
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      26.41

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_F_000             2346
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.787
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6040
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   
;
SADABS 2016/2 Bruker AXS Madison WI USA
;
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX II with Photon 100 CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            111297
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.771
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             18011
_reflns_number_gt                12925
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Structure solved by intrinsic phasing (XT) and residual non-H
atoms located in subsequent difmaps. some disorder evident in
map of the triflate coutnerions and two (part occupancy) MeCN and
two (part occupancy)Et2O molecules located which were refined 
isotropically due to significant disorder. One Et2O molecule removed
in the latter stages of refinement due to persistent residual electron 
density in its vicinity which could not be well modelled. This was
treated with SQUEEZE and then afforded a smooth convergence to R1
= 6.8% and residual electron density < +/- 1.2eA-3.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0794P)²+30.5571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     intrinsic
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18011
_refine_ls_number_parameters     1463
_refine_ls_number_restraints     1959
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.2082
_refine_ls_wR_factor_gt          0.1614
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.46100(5) 0.21429(4) 0.34410(4) 0.02271(18) Uani 1 1 d . U . . .
Fe2 Fe 0.34165(6) 0.35233(4) 0.50113(4) 0.02565(19) Uani 1 1 d . U . . .
Fe3 Fe 0.24108(5) 0.38019(4) 0.22684(4) 0.02109(17) Uani 1 1 d . U . . .
Fe4 Fe 0.36379(5) 0.24327(4) 0.06679(4) 0.02332(18) Uani 1 1 d . U . . .
O1 O 0.4262(3) 0.2531(2) 0.46121(17) 0.0264(8) Uani 1 1 d . U . . .
O2 O 0.4574(3) 0.1931(2) 0.12421(18) 0.0293(8) Uani 1 1 d . U . . .
O3 O 0.2607(2) 0.33111(19) 0.11426(17) 0.0242(7) Uani 1 1 d . U . . .
O4 O 0.2699(3) 0.4170(2) 0.43423(18) 0.0298(8) Uani 1 1 d . U . . .
O5 O 0.2305(3) 0.3112(2) 0.53935(19) 0.0327(9) Uani 1 1 d . U . . .
H5A H 0.2183 0.2837 0.5768 0.039 Uiso 1 1 d R U . . .
H5B H 0.2086 0.2941 0.5126 0.039 Uiso 1 1 d R U . . .
O6 O 0.4477(3) 0.3989(3) 0.4647(2) 0.0377(9) Uani 1 1 d . U . . .
H6A H 0.4985 0.3847 0.4812 0.045 Uiso 1 1 d R U . . .
H6B H 0.4196 0.4471 0.4651 0.045 Uiso 1 1 d R U . . .
O7 O 0.3318(3) 0.1909(2) 0.37884(19) 0.0316(8) Uani 1 1 d . U . . .
H7A H 0.2806 0.2285 0.3885 0.038 Uiso 1 1 d R U . . .
H7B H 0.3210 0.1569 0.3621 0.038 Uiso 1 1 d R U . . .
O8 O 0.2923(3) 0.1694(2) 0.1139(2) 0.0379(9) Uani 1 1 d . U . . .
H8A H 0.3129 0.1312 0.1501 0.045 Uiso 1 1 d R U . . .
H8B H 0.2629 0.1488 0.0885 0.045 Uiso 1 1 d R U . . .
O9 O 0.4428(3) 0.3099(2) 0.01605(19) 0.0330(9) Uani 1 1 d . U . . .
H9A H 0.4201 0.3554 -0.0117 0.040 Uiso 1 1 d R U . . .
H9B H 0.4852 0.2957 0.0004 0.040 Uiso 1 1 d R U . . .
O10 O 0.1961(3) 0.2853(2) 0.2669(2) 0.0346(9) Uani 1 1 d . U . . .
H10A H 0.1739 0.2444 0.2637 0.042 Uiso 1 1 d R U . . .
H10B H 0.1397 0.2901 0.3019 0.042 Uiso 1 1 d R U . . .
N1 N 0.2899(3) 0.4241(3) 0.5847(2) 0.0285(9) Uani 1 1 d . U . . .
N2 N 0.4070(3) 0.2863(3) 0.5818(2) 0.0298(10) Uani 1 1 d . U . . .
N3 N 0.4649(3) 0.2114(3) 0.5712(2) 0.0317(10) Uani 1 1 d . U . . .
N4 N 0.5307(3) 0.1173(2) 0.4168(2) 0.0248(9) Uani 1 1 d . U . . .
N5 N 0.5304(3) 0.1126(2) 0.2861(2) 0.0252(9) Uani 1 1 d . U . . .
N6 N 0.4425(3) 0.2459(2) 0.2255(2) 0.0237(9) Uani 1 1 d . U . . .
N7 N 0.3946(3) 0.3193(2) 0.1949(2) 0.0229(9) Uani 1 1 d . U . . .
N8 N 0.2986(3) 0.4644(3) 0.1629(2) 0.0276(9) Uani 1 1 d . U . . .
N9 N 0.4218(3) 0.1750(3) -0.0200(2) 0.0299(10) Uani 1 1 d . U . . .
N10 N 0.2636(3) 0.2857(2) 0.0024(2) 0.0248(9) Uani 1 1 d . U . . .
N11 N 0.1789(3) 0.3427(2) 0.0260(2) 0.0270(9) Uani 1 1 d . U . . .
N12 N 0.1090(3) 0.4342(2) 0.1824(2) 0.0233(9) Uani 1 1 d . U . . .
N13 N 0.1332(3) 0.4550(2) 0.3022(2) 0.0240(9) Uani 1 1 d . U . . .
N14 N 0.3069(3) 0.3804(2) 0.3223(2) 0.0228(9) Uani 1 1 d . U . . .
N15 N 0.4014(3) 0.3404(2) 0.3309(2) 0.0247(9) Uani 1 1 d . U . . .
N16 N 0.5819(3) 0.2534(3) 0.3248(2) 0.0283(9) Uani 1 1 d . U . . .
C1 C 0.2265(5) 0.4951(3) 0.5836(3) 0.0373(13) Uani 1 1 d . U . . .
H1 H 0.2016 0.5166 0.5424 0.045 Uiso 1 1 calc R U . . .
C2 C 0.1952(5) 0.5388(4) 0.6395(3) 0.0406(14) Uani 1 1 d . U . . .
H2 H 0.1487 0.5887 0.6376 0.049 Uiso 1 1 calc R U . . .
C3 C 0.2345(5) 0.5070(4) 0.6984(3) 0.0392(13) Uani 1 1 d . U . . .
H3 H 0.2147 0.5355 0.7378 0.047 Uiso 1 1 calc R U . . .
C4 C 0.3024(5) 0.4339(4) 0.7005(3) 0.0361(13) Uani 1 1 d . U . . .
H4 H 0.3305 0.4122 0.7404 0.043 Uiso 1 1 calc R U . . .
C5 C 0.3276(4) 0.3937(3) 0.6425(3) 0.0317(12) Uani 1 1 d . U . . .
C6 C 0.3934(4) 0.3136(4) 0.6402(3) 0.0327(12) Uani 1 1 d . U . . .
C7 C 0.4693(4) 0.2009(3) 0.5067(3) 0.0270(11) Uani 1 1 d . U . . .
C8 C 0.5270(4) 0.1238(3) 0.4837(3) 0.0282(11) Uani 1 1 d . U . . .
C9 C 0.5733(5) 0.0640(4) 0.5278(3) 0.0378(14) Uani 1 1 d . U . . .
H9 H 0.5693 0.0706 0.5750 0.045 Uiso 1 1 calc R U . . .
C10 C 0.6259(5) -0.0061(4) 0.5009(3) 0.0419(15) Uani 1 1 d . U . . .
H10 H 0.6586 -0.0484 0.5299 0.050 Uiso 1 1 calc R U . . .
C11 C 0.6309(5) -0.0144(3) 0.4326(3) 0.0379(14) Uani 1 1 d . U . . .
H11 H 0.6668 -0.0621 0.4138 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5821(4) 0.0488(3) 0.3914(3) 0.0282(11) Uani 1 1 d . U . . .
C13 C 0.5842(4) 0.0471(3) 0.3167(3) 0.0290(11) Uani 1 1 d . U . . .
C14 C 0.6389(5) -0.0162(3) 0.2802(3) 0.0384(14) Uani 1 1 d . U . . .
H14 H 0.6760 -0.0620 0.3031 0.046 Uiso 1 1 calc R U . . .
C15 C 0.6387(5) -0.0119(4) 0.2095(3) 0.0474(17) Uani 1 1 d . U . . .
H15 H 0.6770 -0.0539 0.1829 0.057 Uiso 1 1 calc R U . . .
C16 C 0.5809(4) 0.0559(3) 0.1784(3) 0.0347(13) Uani 1 1 d . U . . .
H16 H 0.5784 0.0607 0.1304 0.042 Uiso 1 1 calc R U . . .
C17 C 0.5285(4) 0.1145(3) 0.2181(3) 0.0274(11) Uani 1 1 d . U . . .
C18 C 0.4699(4) 0.1893(3) 0.1874(3) 0.0225(10) Uani 1 1 d . U . . .
C19 C 0.4472(4) 0.3587(3) 0.1594(2) 0.0243(10) Uani 1 1 d . U . . .
C20 C 0.3939(4) 0.4398(3) 0.1365(3) 0.0258(11) Uani 1 1 d . U . . .
C21 C 0.4390(4) 0.4871(3) 0.0932(3) 0.0328(12) Uani 1 1 d . U . . .
H21 H 0.5058 0.4683 0.0752 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3855(5) 0.5628(3) 0.0762(3) 0.0375(13) Uani 1 1 d . U . . .
H22 H 0.4154 0.5968 0.0472 0.045 Uiso 1 1 calc R U . . .
C23 C 0.2892(5) 0.5880(3) 0.1016(3) 0.0401(14) Uani 1 1 d . U . . .
H23 H 0.2512 0.6393 0.0897 0.048 Uiso 1 1 calc R U . . .
C24 C 0.2476(4) 0.5376(3) 0.1451(3) 0.0346(13) Uani 1 1 d . U . . .
H24 H 0.1807 0.5556 0.1629 0.041 Uiso 1 1 calc R U . . .
C25 C 0.5533(4) 0.3313(3) 0.1420(3) 0.0325(12) Uani 1 1 d . U . . .
H25A H 0.5785 0.2820 0.1689 0.049 Uiso 1 1 calc R U . . .
H25B H 0.5768 0.3691 0.1536 0.049 Uiso 1 1 calc R U . . .
H25C H 0.5748 0.3250 0.0921 0.049 Uiso 1 1 calc R U . . .
C26 C 0.4385(5) 0.2698(4) 0.7000(3) 0.0447(16) Uani 1 1 d . U . . .
H26A H 0.4671 0.2153 0.6923 0.067 Uiso 1 1 calc R U . . .
H26B H 0.3899 0.2762 0.7431 0.067 Uiso 1 1 calc R U . . .
H26C H 0.4884 0.2892 0.7041 0.067 Uiso 1 1 calc R U . . .
C27 C 0.5065(5) 0.1181(4) -0.0294(3) 0.0423(15) Uani 1 1 d . U . . .
H27 H 0.5440 0.1038 0.0057 0.051 Uiso 1 1 calc R U . . .
C28 C 0.5407(5) 0.0800(4) -0.0892(4) 0.0534(19) Uani 1 1 d . U . . .
H28 H 0.6015 0.0406 -0.0954 0.064 Uiso 1 1 calc R U . . .
C29 C 0.4852(5) 0.0998(4) -0.1400(3) 0.0488(17) Uani 1 1 d . U . . .
H29 H 0.5069 0.0738 -0.1810 0.059 Uiso 1 1 calc R U . . .
C30 C 0.3982(5) 0.1579(3) -0.1298(3) 0.0373(14) Uani 1 1 d . U . . .
H30 H 0.3591 0.1725 -0.1639 0.045 Uiso 1 1 calc R U . . .
C31 C 0.3682(4) 0.1948(3) -0.0695(3) 0.0282(11) Uani 1 1 d . U . . .
C32 C 0.2749(4) 0.2560(3) -0.0546(3) 0.0300(12) Uani 1 1 d . U . . .
C33 C 0.1856(4) 0.3610(3) 0.0849(3) 0.0228(10) Uani 1 1 d . U . . .
C34 C 0.1023(4) 0.4208(3) 0.1204(3) 0.0244(10) Uani 1 1 d . U . . .
C35 C 0.0220(4) 0.4597(3) 0.0906(3) 0.0290(11) Uani 1 1 d . U . . .
H35 H 0.0185 0.4476 0.0470 0.035 Uiso 1 1 calc R U . . .
C36 C -0.0521(4) 0.5161(3) 0.1257(3) 0.0310(12) Uani 1 1 d . U . . .
H36 H -0.1068 0.5446 0.1058 0.037 Uiso 1 1 calc R U . . .
C37 C -0.0462(4) 0.5310(3) 0.1899(3) 0.0295(12) Uani 1 1 d . U . . .
H37 H -0.0966 0.5698 0.2148 0.035 Uiso 1 1 calc R U . . .
C38 C 0.0356(4) 0.4876(3) 0.2178(3) 0.0243(10) Uani 1 1 d . U . . .
C39 C 0.0471(4) 0.4976(3) 0.2867(3) 0.0237(10) Uani 1 1 d . U . . .
C40 C -0.0220(4) 0.5466(3) 0.3326(3) 0.0313(12) Uani 1 1 d . U . . .
H40 H -0.0820 0.5765 0.3203 0.038 Uiso 1 1 calc R U . . .
C41 C -0.0045(4) 0.5522(3) 0.3958(3) 0.0322(12) Uani 1 1 d . U . . .
H41 H -0.0522 0.5847 0.4280 0.039 Uiso 1 1 calc R U . . .
C42 C 0.0861(4) 0.5086(3) 0.4117(3) 0.0349(13) Uani 1 1 d . U . . .
H42 H 0.1019 0.5124 0.4541 0.042 Uiso 1 1 calc R U . . .
C43 C 0.1507(4) 0.4606(3) 0.3642(3) 0.0243(10) Uani 1 1 d . U . . .
C44 C 0.2491(4) 0.4155(3) 0.3749(3) 0.0231(10) Uani 1 1 d . U . . .
C45 C 0.4603(4) 0.3777(3) 0.3154(3) 0.0253(10) Uani 1 1 d . U . . .
C46 C 0.5619(4) 0.3305(3) 0.3171(3) 0.0285(11) Uani 1 1 d . U . . .
C47 C 0.6326(5) 0.3631(4) 0.3091(4) 0.0471(16) Uani 1 1 d . U . . .
H47 H 0.6171 0.4174 0.3034 0.057 Uiso 1 1 calc R U . . .
C48 C 0.7259(5) 0.3155(4) 0.3097(5) 0.069(2) Uani 1 1 d . U . . .
H48 H 0.7753 0.3367 0.3045 0.083 Uiso 1 1 calc R U . . .
C49 C 0.7463(5) 0.2372(4) 0.3178(5) 0.061(2) Uani 1 1 d . U . . .
H49 H 0.8099 0.2035 0.3182 0.073 Uiso 1 1 calc R U . . .
C50 C 0.6727(4) 0.2085(4) 0.3254(4) 0.0426(14) Uani 1 1 d . U . . .
H50 H 0.6871 0.1543 0.3314 0.051 Uiso 1 1 calc R U . . .
C51 C 0.4355(4) 0.4622(3) 0.2951(3) 0.0303(12) Uani 1 1 d . U . . .
H51A H 0.3704 0.4832 0.2857 0.045 Uiso 1 1 calc R U . . .
H51B H 0.4806 0.4714 0.2530 0.045 Uiso 1 1 calc R U . . .
H51C H 0.4391 0.4873 0.3332 0.045 Uiso 1 1 calc R U . . .
C52 C 0.2046(4) 0.2788(3) -0.1006(3) 0.0363(14) Uani 1 1 d . U . . .
H52A H 0.1444 0.3149 -0.0783 0.054 Uiso 1 1 calc R U . . .
H52B H 0.1934 0.2331 -0.1090 0.054 Uiso 1 1 calc R U . . .
H52C H 0.2294 0.3034 -0.1451 0.054 Uiso 1 1 calc R U . . .
S1A S 0.33572(12) 0.47115(9) 0.88841(8) 0.0389(4) Uani 1 1 d D U . . .
O1A O 0.2942(3) 0.4197(3) 0.8733(2) 0.0492(11) Uani 1 1 d D U . . .
O2A O 0.3850(4) 0.5065(3) 0.8296(2) 0.0574(13) Uani 1 1 d D U . . .
O3A O 0.3845(4) 0.4440(3) 0.9465(2) 0.0505(12) Uani 1 1 d D U . . .
C1A C 0.2343(4) 0.5512(3) 0.9223(3) 0.0486(15) Uani 1 1 d D U . . .
F1A F 0.1787(4) 0.5298(3) 0.9777(3) 0.0764(14) Uani 1 1 d D U . . .
F2A F 0.2636(3) 0.6035(2) 0.9402(2) 0.0608(11) Uani 1 1 d D U . . .
F3A F 0.1805(3) 0.5865(3) 0.8745(3) 0.0761(14) Uani 1 1 d D U . . .
S1B S 0.19928(12) 0.22999(8) 0.71445(7) 0.0365(3) Uani 1 1 d D U . . .
O1B O 0.2339(4) 0.2019(2) 0.6464(2) 0.0466(11) Uani 1 1 d D U . . .
O2B O 0.1929(3) 0.3084(2) 0.7151(2) 0.0425(10) Uani 1 1 d D U . . .
O3B O 0.2409(5) 0.1778(3) 0.7684(2) 0.0689(17) Uani 1 1 d D U . . .
C1B C 0.0760(5) 0.2342(5) 0.7351(5) 0.083(2) Uani 1 1 d D U . . .
F1B F 0.0284(4) 0.2763(4) 0.6871(4) 0.115(2) Uani 1 1 d D U . . .
F2B F 0.0691(5) 0.1652(4) 0.7406(4) 0.131(3) Uani 1 1 d D U . . .
F3B F 0.0322(5) 0.2646(5) 0.7949(4) 0.145(3) Uani 1 1 d D U . . .
S1C S 0.3205(2) 0.0486(2) 0.27549(13) 0.0417(7) Uani 0.815(8) 1 d D U P A 1
O2C O 0.2726(5) 0.1228(4) 0.2945(4) 0.069(2) Uani 0.815(8) 1 d D U P A 1
O3C O 0.3491(8) 0.0446(6) 0.2014(4) 0.059(3) Uani 0.815(8) 1 d D U P A 1
O1C O 0.3964(7) 0.0023(6) 0.3116(5) 0.087(3) Uani 0.815(8) 1 d D U P A 1
S2C S 0.3444(10) 0.0187(9) 0.2862(7) 0.0417(7) Uani 0.185(8) 1 d D U P A 2
O4C O 0.3101(18) 0.0636(11) 0.3444(9) 0.042(5) Uani 0.185(8) 1 d D U P A 2
O5C O 0.4377(19) -0.031(2) 0.2984(18) 0.063(7) Uani 0.185(8) 1 d D U P A 2
O6C O 0.361(4) 0.053(3) 0.2155(15) 0.059(9) Uani 0.185(8) 1 d D U P A 2
C1C C 0.2411(8) -0.0064(7) 0.2996(6) 0.114(3) Uani 1 1 d D U . . .
F1C F 0.2027(8) -0.0063(7) 0.3655(5) 0.195(4) Uani 1 1 d D U . . .
F2C F 0.2857(8) -0.0781(5) 0.2833(6) 0.186(4) Uani 1 1 d D U . . .
F3C F 0.1713(7) 0.0236(7) 0.2669(6) 0.191(4) Uani 1 1 d D U . . .
S1D S 0.05372(11) 0.30300(9) 0.44116(8) 0.0379(4) Uani 1 1 d D U . . .
O1D O 0.0361(4) 0.3065(4) 0.3729(2) 0.0646(15) Uani 1 1 d D U . . .
O2D O -0.0153(3) 0.3575(3) 0.4856(3) 0.0598(14) Uani 1 1 d D U . . .
O3D O 0.1523(3) 0.2938(3) 0.4401(2) 0.0401(10) Uani 1 1 d D U . . .
C1D C 0.0477(6) 0.2100(4) 0.4827(4) 0.077(2) Uani 1 1 d D U . . .
F1D F 0.1159(10) 0.1501(8) 0.4558(12) 0.090(4) Uani 0.64(4) 1 d D U P B 1
F2D F -0.0366(7) 0.2071(9) 0.4763(13) 0.098(4) Uani 0.64(4) 1 d D U P B 1
F3D F 0.049(2) 0.2042(11) 0.5496(5) 0.114(5) Uani 0.64(4) 1 d D U P B 1
F4D F 0.104(2) 0.1620(15) 0.4333(15) 0.088(7) Uani 0.36(4) 1 d D U P B 2
F5D F -0.0321(13) 0.1977(15) 0.5076(18) 0.089(6) Uani 0.36(4) 1 d D U P B 2
F6D F 0.093(2) 0.1890(18) 0.5396(11) 0.095(6) Uani 0.36(4) 1 d D U P B 2
S1F S 0.6114(3) 0.3832(2) 0.5696(2) 0.0321(14) Uani 0.613(16) 1 d D U P C 1
O1F O 0.5935(7) 0.3333(6) 0.5312(6) 0.052(3) Uani 0.613(16) 1 d D U P C 1
O2F O 0.6112(8) 0.4549(5) 0.5300(6) 0.060(3) Uani 0.613(16) 1 d D U P C 1
O3F O 0.5647(12) 0.3863(10) 0.6404(5) 0.091(5) Uani 0.613(16) 1 d D U P C 1
C1F C 0.7374(7) 0.3374(7) 0.5720(8) 0.094(4) Uani 0.613(16) 1 d D U P C 1
F1F F 0.7662(10) 0.3820(8) 0.6007(11) 0.148(6) Uani 0.613(16) 1 d D U P C 1
F2F F 0.7881(7) 0.3270(7) 0.5067(8) 0.127(5) Uani 0.613(16) 1 d D U P C 1
F3F F 0.7541(10) 0.2687(6) 0.6082(9) 0.130(5) Uani 0.613(16) 1 d D U P C 1
S1I S 0.6152(10) 0.3847(8) 0.5672(8) 0.096(5) Uani 0.387(16) 1 d D U P C 2
O1I O 0.620(2) 0.3402(17) 0.5140(14) 0.129(10) Uani 0.387(16) 1 d D U P C 2
O2I O 0.6501(17) 0.4484(11) 0.5465(14) 0.109(7) Uani 0.387(16) 1 d D U P C 2
O3I O 0.5323(14) 0.4011(17) 0.6214(13) 0.113(8) Uani 0.387(16) 1 d D U P C 2
C1I C 0.7121(13) 0.3250(11) 0.6108(11) 0.121(6) Uani 0.387(16) 1 d D U P C 2
F1I F 0.7259(16) 0.3642(13) 0.6537(13) 0.135(7) Uani 0.387(16) 1 d D U P C 2
F2I F 0.693(2) 0.2634(11) 0.6426(13) 0.155(8) Uani 0.387(16) 1 d D U P C 2
F3I F 0.7917(11) 0.3064(14) 0.5622(13) 0.124(7) Uani 0.387(16) 1 d D U P C 2
S1G S 0.2134(5) 0.0664(5) 0.0023(4) 0.0524(16) Uani 0.580(9) 1 d D U P D 1
O1G O 0.1994(16) 0.1330(8) 0.0359(11) 0.064(5) Uani 0.580(9) 1 d D U P D 1
O2G O 0.2998(9) 0.0054(9) 0.0012(9) 0.108(5) Uani 0.580(9) 1 d D U P D 1
O3G O 0.1866(10) 0.0901(7) -0.0646(5) 0.092(4) Uani 0.580(9) 1 d D U P D 1
C1G C 0.1282(10) 0.0254(8) 0.0574(8) 0.115(5) Uani 0.580(9) 1 d D U P D 1
F1G F 0.0433(9) 0.0754(8) 0.0700(10) 0.150(6) Uani 0.580(9) 1 d D U P D 1
F2G F 0.1192(11) -0.0302(8) 0.0300(9) 0.159(6) Uani 0.580(9) 1 d D U P D 1
F3G F 0.1504(13) 0.0016(11) 0.1197(8) 0.182(6) Uani 0.580(9) 1 d D U P D 1
S1H S 0.2199(9) 0.0526(8) 0.0177(6) 0.071(3) Uani 0.420(9) 1 d D U P D 2
O1H O 0.207(3) 0.1282(13) 0.0326(19) 0.090(9) Uani 0.420(9) 1 d D U P D 2
O2H O 0.3028(13) 0.0195(14) -0.0321(10) 0.107(7) Uani 0.420(9) 1 d D U P D 2
O3H O 0.2099(15) 0.0008(10) 0.0791(8) 0.109(6) Uani 0.420(9) 1 d D U P D 2
C1H C 0.1245(12) 0.0653(10) -0.0254(9) 0.109(5) Uani 0.420(9) 1 d D U P D 2
F1H F 0.0393(11) 0.0997(13) 0.0104(11) 0.150(7) Uani 0.420(9) 1 d D U P D 2
F2H F 0.1319(14) 0.1089(10) -0.0849(9) 0.128(6) Uani 0.420(9) 1 d D U P D 2
F3H F 0.1213(15) -0.0005(10) -0.0383(12) 0.146(7) Uani 0.420(9) 1 d D U P D 2
N1S N 0.0651(13) 0.6626(15) 1.0738(12) 0.124(8) Uani 0.5 1 d D U P . .
C6S C 0.0457(14) 0.6977(15) 1.0249(14) 0.101(7) Uani 0.5 1 d D U P . .
C7S C 0.0201(15) 0.7318(13) 0.9598(12) 0.095(6) Uani 0.5 1 d D U P . .
H7SA H 0.0723 0.7479 0.9299 0.143 Uiso 0.5 1 calc R U P . .
H7SB H -0.0381 0.7767 0.9672 0.143 Uiso 0.5 1 calc R U P . .
H7SC H 0.0086 0.6944 0.9373 0.143 Uiso 0.5 1 calc R U P . .
N2S N 0.9465(6) 0.3333(5) 0.2311(5) 0.085(2) Uani 1 1 d D . . . .
C8SB C 0.981(3) 0.292(2) 0.1914(19) 0.084(10) Uiso 0.3 1 d D . P E 2
C9SB C 1.018(5) 0.230(3) 0.150(3) 0.19(3) Uiso 0.3 1 d D . P E 2
H9SA H 1.0884 0.2120 0.1410 0.291 Uiso 0.3 1 calc . U P F 2
H9SB H 0.9964 0.2460 0.1052 0.291 Uiso 0.3 1 calc . U P G 2
H9SC H 0.9960 0.1873 0.1743 0.291 Uiso 0.3 1 calc . U P H 2
C9SA C 1.046(2) 0.1888(17) 0.2327(16) 0.190(12) Uiso 0.7 1 d . . P E 1
H9SD H 1.0898 0.1751 0.1881 0.286 Uiso 0.7 1 calc R U P E 1
H9SE H 1.0034 0.1585 0.2447 0.286 Uiso 0.7 1 calc R U P E 1
H9SF H 1.0839 0.1778 0.2693 0.286 Uiso 0.7 1 calc R U P E 1
C8SA C 0.9885(11) 0.2732(9) 0.2267(8) 0.073(4) Uiso 0.7 1 d . . P E 1
C91 C 0.879(3) 0.031(3) 1.2689(16) 0.41(2) Uiso 1 1 d D . . . .
H91A H 0.9212 -0.0068 1.2364 0.611 Uiso 1 1 calc . U . . .
H91B H 0.8889 0.0804 1.2536 0.611 Uiso 1 1 calc . U . . .
H91C H 0.8120 0.0371 1.2695 0.611 Uiso 1 1 calc . U . . .
C92 C 0.901(2) 0.0026(15) 1.3428(17) 0.310(16) Uiso 1 1 d D . . . .
H92A H 0.8879 -0.0467 1.3564 0.372 Uiso 1 1 calc R U . . .
H92B H 0.9702 -0.0096 1.3384 0.372 Uiso 1 1 calc R U . . .
O93 O 0.8554(17) 0.0470(14) 1.3999(14) 0.322(11) Uiso 1 1 d D . . . .
C94 C 0.846(2) 0.0696(17) 1.4653(15) 0.290(15) Uiso 1 1 d D . . . .
H94A H 0.9088 0.0745 1.4653 0.348 Uiso 1 1 calc R U . . .
H94B H 0.8416 0.0250 1.4991 0.348 Uiso 1 1 calc R U . . .
C95 C 0.770(2) 0.1409(19) 1.4987(16) 0.36(2) Uiso 1 1 d D . . . .
H95A H 0.7642 0.1329 1.5494 0.541 Uiso 1 1 calc R U . . .
H95B H 0.7079 0.1486 1.4871 0.541 Uiso 1 1 calc R U . . .
H95C H 0.7885 0.1865 1.4805 0.541 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O7 2.105(4) . ?
Fe1 N16 2.153(5) . ?
Fe1 N5 2.190(4) . ?
Fe1 N15 2.198(4) . ?
Fe1 N4 2.226(4) . ?
Fe1 N6 2.385(4) . ?
Fe2 O4 1.902(4) . ?
Fe2 O1 2.010(4) . ?
Fe2 O6 2.036(4) . ?
Fe2 O5 2.043(4) . ?
Fe2 N2 2.069(4) . ?
Fe2 N1 2.135(4) . ?
Fe3 O10 2.097(4) . ?
Fe3 N8 2.154(5) . ?
Fe3 N13 2.189(4) . ?
Fe3 N7 2.193(4) . ?
Fe3 N12 2.226(4) . ?
Fe3 N14 2.352(4) . ?
Fe4 O2 1.917(4) . ?
Fe4 O3 2.007(3) . ?
Fe4 O9 2.023(4) . ?
Fe4 O8 2.034(4) . ?
Fe4 N10 2.079(4) . ?
Fe4 N9 2.145(4) . ?
O1 C7 1.312(6) . ?
O2 C18 1.299(6) . ?
O3 C33 1.311(6) . ?
O4 C44 1.298(6) . ?
O5 H5A 0.8501 . ?
O5 H5B 0.8495 . ?
O6 H6A 0.8501 . ?
O6 H6B 0.8500 . ?
O7 H7A 0.8500 . ?
O7 H7B 0.8498 . ?
O8 H8A 0.9461 . ?
O8 H8B 0.9522 . ?
O9 H9A 0.9306 . ?
O9 H9B 0.6275 . ?
O10 H10A 0.9613 . ?
O10 H10B 0.9540 . ?
N1 C1 1.333(8) . ?
N1 C5 1.353(7) . ?
N2 C6 1.290(7) . ?
N2 N3 1.383(7) . ?
N3 C7 1.311(7) . ?
N4 C8 1.341(7) . ?
N4 C12 1.350(7) . ?
N5 C13 1.344(7) . ?
N5 C17 1.350(7) . ?
N6 C18 1.295(6) . ?
N6 N7 1.412(6) . ?
N7 C19 1.288(7) . ?
N8 C24 1.345(7) . ?
N8 C20 1.356(7) . ?
N9 C27 1.343(7) . ?
N9 C31 1.350(7) . ?
N10 C32 1.295(7) . ?
N10 N11 1.385(6) . ?
N11 C33 1.310(7) . ?
N12 C34 1.331(6) . ?
N12 C38 1.344(7) . ?
N13 C39 1.348(7) . ?
N13 C43 1.349(7) . ?
N14 C44 1.295(7) . ?
N14 N15 1.404(6) . ?
N15 C45 1.281(7) . ?
N16 C50 1.340(8) . ?
N16 C46 1.355(7) . ?
C1 C2 1.381(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.385(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.476(9) . ?
C6 C26 1.485(8) . ?
C7 C8 1.480(8) . ?
C8 C9 1.380(8) . ?
C9 C10 1.391(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.371(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.481(7) . ?
C13 C14 1.387(8) . ?
C14 C15 1.392(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.397(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.354(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.483(7) . ?
C19 C25 1.485(8) . ?
C19 C20 1.492(7) . ?
C20 C21 1.376(8) . ?
C21 C22 1.387(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.365(9) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.385(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.376(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.382(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.473(8) . ?
C32 C52 1.474(8) . ?
C33 C34 1.478(7) . ?
C34 C35 1.393(7) . ?
C35 C36 1.377(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.382(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.404(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.472(7) . ?
C39 C40 1.383(7) . ?
C40 C41 1.372(8) . ?
C40 H40 0.9500 . ?
C41 C42 1.410(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.369(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.482(7) . ?
C45 C46 1.489(8) . ?
C45 C51 1.494(7) . ?
C46 C47 1.388(8) . ?
C47 C48 1.384(10) . ?
C47 H47 0.9500 . ?
C48 C49 1.374(10) . ?
C48 H48 0.9500 . ?
C49 C50 1.381(9) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
S1A O2A 1.426(4) . ?
S1A O1A 1.434(4) . ?
S1A O3A 1.443(4) . ?
S1A C1A 1.810(6) . ?
C1A F1A 1.316(7) . ?
C1A F3A 1.334(7) . ?
C1A F2A 1.342(6) . ?
S1B O3B 1.422(4) . ?
S1B O2B 1.440(4) . ?
S1B O1B 1.443(4) . ?
S1B C1B 1.804(7) . ?
C1B F1B 1.310(9) . ?
C1B F2B 1.321(8) . ?
C1B F3B 1.325(8) . ?
S1C O2C 1.388(6) . ?
S1C O3C 1.437(7) . ?
S1C O1C 1.439(8) . ?
S1C C1C 1.795(9) . ?
S2C O4C 1.430(11) . ?
S2C O6C 1.444(19) . ?
S2C O5C 1.448(18) . ?
S2C C1C 1.754(13) . ?
C1C F3C 1.285(10) . ?
C1C F1C 1.296(10) . ?
C1C F2C 1.325(10) . ?
S1D O2D 1.422(4) . ?
S1D O1D 1.431(5) . ?
S1D O3D 1.448(4) . ?
S1D C1D 1.819(7) . ?
C1D F5D 1.289(14) . ?
C1D F1D 1.314(10) . ?
C1D F3D 1.319(10) . ?
C1D F2D 1.347(10) . ?
C1D F4D 1.360(15) . ?
C1D F6D 1.388(15) . ?
S1F O3F 1.413(8) . ?
S1F O2F 1.433(7) . ?
S1F O1F 1.437(7) . ?
S1F C1F 1.812(9) . ?
C1F F1F 1.330(11) . ?
C1F F3F 1.331(10) . ?
C1F F2F 1.344(11) . ?
S1I O3I 1.425(11) . ?
S1I O1I 1.427(11) . ?
S1I O2I 1.437(11) . ?
S1I C1I 1.811(11) . ?
C1I F2I 1.312(12) . ?
C1I F1I 1.313(12) . ?
C1I F3I 1.333(12) . ?
S1G O2G 1.399(9) . ?
S1G O3G 1.433(10) . ?
S1G O1G 1.441(9) . ?
S1G C1G 1.797(10) . ?
C1G F1G 1.292(11) . ?
C1G F2G 1.318(11) . ?
C1G F3G 1.320(11) . ?
S1H O2H 1.418(11) . ?
S1H O1H 1.433(10) . ?
S1H O3H 1.434(11) . ?
S1H C1H 1.788(11) . ?
C1H F1H 1.312(12) . ?
C1H F2H 1.320(12) . ?
C1H F3H 1.322(11) . ?
N1S C6S 1.11(2) . ?
C6S C7S 1.42(3) . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
N2S C8SA 1.083(16) . ?
N2S C8SB 1.10(3) . ?
C8SB C9SB 1.42(3) . ?
C9SB H9SA 0.9800 . ?
C9SB H9SB 0.9800 . ?
C9SB H9SC 0.9800 . ?
C9SA C8SA 1.51(3) . ?
C9SA H9SD 0.9800 . ?
C9SA H9SE 0.9800 . ?
C9SA H9SF 0.9800 . ?
C91 C92 1.544(10) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
C92 O93 1.409(10) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
O93 C94 1.396(10) . ?
C94 C95 1.549(10) . ?
C94 H94A 0.9900 . ?
C94 H94B 0.9900 . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Fe1 N16 168.58(16) . . ?
O7 Fe1 N5 93.41(16) . . ?
N16 Fe1 N5 97.55(17) . . ?
O7 Fe1 N15 98.52(16) . . ?
N16 Fe1 N15 74.50(17) . . ?
N5 Fe1 N15 142.88(16) . . ?
O7 Fe1 N4 90.27(15) . . ?
N16 Fe1 N4 89.99(16) . . ?
N5 Fe1 N4 72.51(16) . . ?
N15 Fe1 N4 141.87(16) . . ?
O7 Fe1 N6 94.30(15) . . ?
N16 Fe1 N6 92.54(16) . . ?
N5 Fe1 N6 69.37(15) . . ?
N15 Fe1 N6 74.76(15) . . ?
N4 Fe1 N6 141.79(15) . . ?
O4 Fe2 O1 109.23(15) . . ?
O4 Fe2 O6 91.20(17) . . ?
O1 Fe2 O6 90.84(16) . . ?
O4 Fe2 O5 87.54(17) . . ?
O1 Fe2 O5 92.21(16) . . ?
O6 Fe2 O5 176.94(17) . . ?
O4 Fe2 N2 173.99(17) . . ?
O1 Fe2 N2 75.56(16) . . ?
O6 Fe2 N2 92.38(18) . . ?
O5 Fe2 N2 88.64(17) . . ?
O4 Fe2 N1 100.34(17) . . ?
O1 Fe2 N1 150.43(16) . . ?
O6 Fe2 N1 88.61(17) . . ?
O5 Fe2 N1 88.87(16) . . ?
N2 Fe2 N1 74.93(18) . . ?
O10 Fe3 N8 166.23(16) . . ?
O10 Fe3 N13 93.67(16) . . ?
N8 Fe3 N13 98.61(16) . . ?
O10 Fe3 N7 99.00(16) . . ?
N8 Fe3 N7 74.43(16) . . ?
N13 Fe3 N7 144.37(16) . . ?
O10 Fe3 N12 88.71(16) . . ?
N8 Fe3 N12 89.07(16) . . ?
N13 Fe3 N12 72.41(15) . . ?
N7 Fe3 N12 140.56(15) . . ?
O10 Fe3 N14 96.37(15) . . ?
N8 Fe3 N14 93.69(16) . . ?
N13 Fe3 N14 69.99(15) . . ?
N7 Fe3 N14 75.57(15) . . ?
N12 Fe3 N14 142.29(15) . . ?
O2 Fe4 O3 109.42(15) . . ?
O2 Fe4 O9 89.45(16) . . ?
O3 Fe4 O9 92.99(15) . . ?
O2 Fe4 O8 89.22(17) . . ?
O3 Fe4 O8 91.49(16) . . ?
O9 Fe4 O8 175.52(17) . . ?
O2 Fe4 N10 173.67(16) . . ?
O3 Fe4 N10 75.35(15) . . ?
O9 Fe4 N10 94.51(17) . . ?
O8 Fe4 N10 86.46(17) . . ?
O2 Fe4 N9 100.86(16) . . ?
O3 Fe4 N9 149.72(16) . . ?
O9 Fe4 N9 87.64(17) . . ?
O8 Fe4 N9 88.41(18) . . ?
N10 Fe4 N9 74.42(17) . . ?
C7 O1 Fe2 113.6(3) . . ?
C18 O2 Fe4 140.9(3) . . ?
C33 O3 Fe4 113.9(3) . . ?
C44 O4 Fe2 141.1(3) . . ?
Fe2 O5 H5A 131.1 . . ?
Fe2 O5 H5B 120.9 . . ?
H5A O5 H5B 98.9 . . ?
Fe2 O6 H6A 123.5 . . ?
Fe2 O6 H6B 105.0 . . ?
H6A O6 H6B 110.9 . . ?
Fe1 O7 H7A 117.9 . . ?
Fe1 O7 H7B 121.7 . . ?
H7A O7 H7B 110.5 . . ?
Fe4 O8 H8A 122.6 . . ?
Fe4 O8 H8B 122.0 . . ?
H8A O8 H8B 106.4 . . ?
Fe4 O9 H9A 124.7 . . ?
Fe4 O9 H9B 121.9 . . ?
H9A O9 H9B 102.7 . . ?
Fe3 O10 H10A 154.2 . . ?
Fe3 O10 H10B 121.1 . . ?
H10A O10 H10B 72.9 . . ?
C1 N1 C5 118.8(5) . . ?
C1 N1 Fe2 125.8(4) . . ?
C5 N1 Fe2 115.4(4) . . ?
C6 N2 N3 121.1(5) . . ?
C6 N2 Fe2 121.2(4) . . ?
N3 N2 Fe2 117.6(3) . . ?
C7 N3 N2 107.7(4) . . ?
C8 N4 C12 118.3(4) . . ?
C8 N4 Fe1 123.6(4) . . ?
C12 N4 Fe1 118.1(3) . . ?
C13 N5 C17 117.7(5) . . ?
C13 N5 Fe1 119.5(3) . . ?
C17 N5 Fe1 122.5(3) . . ?
C18 N6 N7 116.5(4) . . ?
C18 N6 Fe1 117.0(3) . . ?
N7 N6 Fe1 126.1(3) . . ?
C19 N7 N6 116.7(4) . . ?
C19 N7 Fe3 117.9(3) . . ?
N6 N7 Fe3 123.2(3) . . ?
C24 N8 C20 117.9(5) . . ?
C24 N8 Fe3 125.6(4) . . ?
C20 N8 Fe3 116.5(3) . . ?
C27 N9 C31 119.2(5) . . ?
C27 N9 Fe4 125.6(4) . . ?
C31 N9 Fe4 115.1(3) . . ?
C32 N10 N11 120.3(4) . . ?
C32 N10 Fe4 122.1(4) . . ?
N11 N10 Fe4 117.4(3) . . ?
C33 N11 N10 107.7(4) . . ?
C34 N12 C38 118.9(4) . . ?
C34 N12 Fe3 123.3(3) . . ?
C38 N12 Fe3 117.5(3) . . ?
C39 N13 C43 118.4(4) . . ?
C39 N13 Fe3 119.8(3) . . ?
C43 N13 Fe3 121.8(3) . . ?
C44 N14 N15 116.1(4) . . ?
C44 N14 Fe3 117.3(3) . . ?
N15 N14 Fe3 126.4(3) . . ?
C45 N15 N14 117.7(4) . . ?
C45 N15 Fe1 117.6(4) . . ?
N14 N15 Fe1 122.9(3) . . ?
C50 N16 C46 117.9(5) . . ?
C50 N16 Fe1 125.7(4) . . ?
C46 N16 Fe1 116.2(4) . . ?
N1 C1 C2 123.3(6) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 117.4(6) . . ?
C1 C2 H2 121.3 . . ?
C3 C2 H2 121.3 . . ?
C2 C3 C4 120.7(5) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 117.7(5) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
N1 C5 C4 122.1(6) . . ?
N1 C5 C6 114.9(5) . . ?
C4 C5 C6 122.9(5) . . ?
N2 C6 C5 113.4(5) . . ?
N2 C6 C26 124.2(6) . . ?
C5 C6 C26 122.5(5) . . ?
N3 C7 O1 125.1(5) . . ?
N3 C7 C8 117.3(5) . . ?
O1 C7 C8 117.6(4) . . ?
N4 C8 C9 123.2(5) . . ?
N4 C8 C7 114.4(4) . . ?
C9 C8 C7 122.4(5) . . ?
C8 C9 C10 117.8(5) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 118.5(6) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
N4 C12 C11 122.0(5) . . ?
N4 C12 C13 114.8(5) . . ?
C11 C12 C13 123.2(5) . . ?
N5 C13 C14 122.1(5) . . ?
N5 C13 C12 114.8(5) . . ?
C14 C13 C12 123.1(5) . . ?
C13 C14 C15 119.2(5) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C14 C15 C16 118.4(6) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
C17 C16 C15 118.7(5) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
N5 C17 C16 123.9(5) . . ?
N5 C17 C18 114.7(4) . . ?
C16 C17 C18 121.2(5) . . ?
N6 C18 O2 126.8(5) . . ?
N6 C18 C17 115.1(4) . . ?
O2 C18 C17 117.9(4) . . ?
N7 C19 C25 126.2(5) . . ?
N7 C19 C20 115.2(5) . . ?
C25 C19 C20 118.6(5) . . ?
N8 C20 C21 122.3(5) . . ?
N8 C20 C19 115.5(5) . . ?
C21 C20 C19 122.2(5) . . ?
C20 C21 C22 119.0(6) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
C23 C22 C21 119.3(6) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 119.2(6) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
N8 C24 C23 122.4(6) . . ?
N8 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C19 C25 H25A 109.5 . . ?
C19 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C19 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C6 C26 H26A 109.5 . . ?
C6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N9 C27 C28 121.6(6) . . ?
N9 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C29 119.3(6) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 118.8(6) . . ?
C30 C29 H29 120.6 . . ?
C28 C29 H29 120.6 . . ?
C29 C30 C31 119.5(6) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
N9 C31 C30 121.6(5) . . ?
N9 C31 C32 116.1(4) . . ?
C30 C31 C32 122.2(5) . . ?
N10 C32 C31 112.0(5) . . ?
N10 C32 C52 125.6(5) . . ?
C31 C32 C52 122.4(5) . . ?
N11 C33 O3 125.1(5) . . ?
N11 C33 C34 117.4(4) . . ?
O3 C33 C34 117.5(4) . . ?
N12 C34 C35 122.8(5) . . ?
N12 C34 C33 115.8(4) . . ?
C35 C34 C33 121.5(5) . . ?
C36 C35 C34 118.5(5) . . ?
C36 C35 H35 120.8 . . ?
C34 C35 H35 120.8 . . ?
C35 C36 C37 119.5(5) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C36 C37 C38 118.7(5) . . ?
C36 C37 H37 120.6 . . ?
C38 C37 H37 120.6 . . ?
N12 C38 C37 121.5(5) . . ?
N12 C38 C39 115.8(4) . . ?
C37 C38 C39 122.7(5) . . ?
N13 C39 C40 121.3(5) . . ?
N13 C39 C38 114.0(4) . . ?
C40 C39 C38 124.7(5) . . ?
C41 C40 C39 120.4(5) . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C40 C41 C42 118.4(5) . . ?
C40 C41 H41 120.8 . . ?
C42 C41 H41 120.8 . . ?
C43 C42 C41 118.1(5) . . ?
C43 C42 H42 121.0 . . ?
C41 C42 H42 121.0 . . ?
N13 C43 C42 123.4(5) . . ?
N13 C43 C44 114.6(4) . . ?
C42 C43 C44 121.8(5) . . ?
N14 C44 O4 126.6(5) . . ?
N14 C44 C43 115.7(4) . . ?
O4 C44 C43 117.7(4) . . ?
N15 C45 C46 115.4(5) . . ?
N15 C45 C51 125.7(5) . . ?
C46 C45 C51 118.9(5) . . ?
N16 C46 C47 121.8(5) . . ?
N16 C46 C45 115.7(5) . . ?
C47 C46 C45 122.4(5) . . ?
C48 C47 C46 119.1(6) . . ?
C48 C47 H47 120.4 . . ?
C46 C47 H47 120.4 . . ?
C49 C48 C47 119.2(7) . . ?
C49 C48 H48 120.4 . . ?
C47 C48 H48 120.4 . . ?
C48 C49 C50 118.9(7) . . ?
C48 C49 H49 120.6 . . ?
C50 C49 H49 120.6 . . ?
N16 C50 C49 123.1(6) . . ?
N16 C50 H50 118.5 . . ?
C49 C50 H50 118.5 . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C32 C52 H52A 109.5 . . ?
C32 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C32 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O2A S1A O1A 116.0(3) . . ?
O2A S1A O3A 114.3(3) . . ?
O1A S1A O3A 114.8(3) . . ?
O2A S1A C1A 103.2(3) . . ?
O1A S1A C1A 104.6(3) . . ?
O3A S1A C1A 101.5(3) . . ?
F1A C1A F3A 107.3(5) . . ?
F1A C1A F2A 107.9(5) . . ?
F3A C1A F2A 107.4(5) . . ?
F1A C1A S1A 112.4(4) . . ?
F3A C1A S1A 110.9(4) . . ?
F2A C1A S1A 110.7(4) . . ?
O3B S1B O2B 115.0(3) . . ?
O3B S1B O1B 114.2(3) . . ?
O2B S1B O1B 114.4(3) . . ?
O3B S1B C1B 104.3(4) . . ?
O2B S1B C1B 103.6(3) . . ?
O1B S1B C1B 103.5(4) . . ?
F1B C1B F2B 106.9(8) . . ?
F1B C1B F3B 107.4(8) . . ?
F2B C1B F3B 108.3(8) . . ?
F1B C1B S1B 112.1(6) . . ?
F2B C1B S1B 111.4(6) . . ?
F3B C1B S1B 110.5(6) . . ?
O2C S1C O3C 113.7(6) . . ?
O2C S1C O1C 116.1(5) . . ?
O3C S1C O1C 112.0(6) . . ?
O2C S1C C1C 110.0(5) . . ?
O3C S1C C1C 102.3(6) . . ?
O1C S1C C1C 101.1(6) . . ?
O4C S2C O6C 122(3) . . ?
O4C S2C O5C 102(2) . . ?
O6C S2C O5C 105(3) . . ?
O4C S2C C1C 94.2(12) . . ?
O6C S2C C1C 109(2) . . ?
O5C S2C C1C 126.7(18) . . ?
F3C C1C F1C 106.0(11) . . ?
F3C C1C F2C 107.8(10) . . ?
F1C C1C F2C 109.9(11) . . ?
F3C C1C S2C 127.3(10) . . ?
F1C C1C S2C 108.7(9) . . ?
F2C C1C S2C 96.2(9) . . ?
F3C C1C S1C 109.9(8) . . ?
F1C C1C S1C 111.9(8) . . ?
F2C C1C S1C 111.2(8) . . ?
O2D S1D O1D 116.7(3) . . ?
O2D S1D O3D 114.8(3) . . ?
O1D S1D O3D 112.3(3) . . ?
O2D S1D C1D 105.2(3) . . ?
O1D S1D C1D 104.3(4) . . ?
O3D S1D C1D 101.3(3) . . ?
F1D C1D F3D 107.8(10) . . ?
F1D C1D F2D 108.1(10) . . ?
F3D C1D F2D 108.6(9) . . ?
F5D C1D F4D 111.6(17) . . ?
F5D C1D F6D 103.1(13) . . ?
F4D C1D F6D 106.9(15) . . ?
F5D C1D S1D 122.6(13) . . ?
F1D C1D S1D 115.4(10) . . ?
F3D C1D S1D 110.2(8) . . ?
F2D C1D S1D 106.6(9) . . ?
F4D C1D S1D 102.4(13) . . ?
F6D C1D S1D 109.5(13) . . ?
O3F S1F O2F 116.8(8) . . ?
O3F S1F O1F 116.0(8) . . ?
O2F S1F O1F 112.5(7) . . ?
O3F S1F C1F 105.0(8) . . ?
O2F S1F C1F 101.1(6) . . ?
O1F S1F C1F 102.8(6) . . ?
F1F C1F F3F 109.7(12) . . ?
F1F C1F F2F 109.5(12) . . ?
F3F C1F F2F 107.5(12) . . ?
F1F C1F S1F 109.2(9) . . ?
F3F C1F S1F 111.2(9) . . ?
F2F C1F S1F 109.7(8) . . ?
O3I S1I O1I 118.4(16) . . ?
O3I S1I O2I 112.1(15) . . ?
O1I S1I O2I 117.7(16) . . ?
O3I S1I C1I 104.8(13) . . ?
O1I S1I C1I 104.0(14) . . ?
O2I S1I C1I 95.6(12) . . ?
F2I C1I F1I 112.6(17) . . ?
F2I C1I F3I 111.0(17) . . ?
F1I C1I F3I 106.6(16) . . ?
F2I C1I S1I 108.8(14) . . ?
F1I C1I S1I 110.3(13) . . ?
F3I C1I S1I 107.4(12) . . ?
O2G S1G O3G 113.5(10) . . ?
O2G S1G O1G 118.6(11) . . ?
O3G S1G O1G 109.8(10) . . ?
O2G S1G C1G 102.7(9) . . ?
O3G S1G C1G 107.7(9) . . ?
O1G S1G C1G 103.3(10) . . ?
F1G C1G F2G 105.8(13) . . ?
F1G C1G F3G 103.9(14) . . ?
F2G C1G F3G 111.2(14) . . ?
F1G C1G S1G 112.4(10) . . ?
F2G C1G S1G 113.0(10) . . ?
F3G C1G S1G 110.1(11) . . ?
O2H S1H O1H 115.2(17) . . ?
O2H S1H O3H 112.0(13) . . ?
O1H S1H O3H 113.4(16) . . ?
O2H S1H C1H 103.1(12) . . ?
O1H S1H C1H 104.9(14) . . ?
O3H S1H C1H 107.1(11) . . ?
F1H C1H F2H 105.3(16) . . ?
F1H C1H F3H 105.2(15) . . ?
F2H C1H F3H 108.5(15) . . ?
F1H C1H S1H 113.8(12) . . ?
F2H C1H S1H 110.8(12) . . ?
F3H C1H S1H 112.8(12) . . ?
N1S C6S C7S 171(3) . . ?
C6S C7S H7SA 109.5 . . ?
C6S C7S H7SB 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
C6S C7S H7SC 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
N2S C8SB C9SB 169(5) . . ?
C8SB C9SB H9SA 109.5 . . ?
C8SB C9SB H9SB 109.5 . . ?
H9SA C9SB H9SB 109.5 . . ?
C8SB C9SB H9SC 109.5 . . ?
H9SA C9SB H9SC 109.5 . . ?
H9SB C9SB H9SC 109.5 . . ?
C8SA C9SA H9SD 109.5 . . ?
C8SA C9SA H9SE 109.5 . . ?
H9SD C9SA H9SE 109.5 . . ?
C8SA C9SA H9SF 109.5 . . ?
H9SD C9SA H9SF 109.5 . . ?
H9SE C9SA H9SF 109.5 . . ?
N2S C8SA C9SA 171(2) . . ?
C92 C91 H91A 109.5 . . ?
C92 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C92 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
O93 C92 C91 122.8(18) . . ?
O93 C92 H92A 106.6 . . ?
C91 C92 H92A 106.6 . . ?
O93 C92 H92B 106.6 . . ?
C91 C92 H92B 106.6 . . ?
H92A C92 H92B 106.6 . . ?
C94 O93 C92 155(2) . . ?
O93 C94 C95 127.1(18) . . ?
O93 C94 H94A 105.5 . . ?
C95 C94 H94A 105.5 . . ?
O93 C94 H94B 105.5 . . ?
C95 C94 H94B 105.5 . . ?
H94A C94 H94B 106.1 . . ?
C94 C95 H95A 109.5 . . ?
C94 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
C94 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?

_refine_diff_density_max         1.149
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.112



